Preparation of a quartz glass body in a multi-chamber oven

ABSTRACT

One aspect relates to a process for the preparation of a quartz glass body, including providing a silicon dioxide granulate, wherein the silicon dioxide granulate was made from pyrogenic silicon dioxide powder and the silicon dioxide granulate has a BET surface area in a range from 20 to 40 m2/g, making a glass melt out of silicon dioxide granulate in an oven and making a quartz glass body out of at least part of the glass melt. The oven has at least a first and a further chamber connected to one another via a passage. The temperature in the first chamber is lower than the temperature in the further chambers. On aspect relates to a quartz glass body which is obtainable by this process. One aspect relates to a light guide, an illuminant and a formed body, which are each obtainable by further processing of the quartz glass body.

CROSS REFERENCE TO RELATED APPLICATION

This Utility Patent Application is a continuation application of U.S.Ser. No. 16/061,929, filed Nov. 9, 2018 and claims the benefit of thefiling date of European Application No. 15201097.1, filed Dec. 18, 2015,and International Application No. PCT/EP2016/081519, filed Dec. 16,2016, all of which are herein incorporated by reference.

The invention relates to a process for the preparation of a quartz glassbody comprising the process steps i.) Providing a silicon dioxidegranulate, wherein the silicon dioxide granulate was prepared frompyrogenic silicon dioxide powder and the silicon dioxide granulate has aBET surface area in a range from 20 to 40 m²/g, ii.) Making a glass meltout of the silicon dioxide granulate in an oven and iii) Making a quartzglass body out of at least a part of the glass melt, wherein the ovenhas at least a first and a further chamber connected to one another viaa passage, wherein the temperature in the first chamber is lower thanthe temperature in the further chamber. Furthermore, the inventionrelates to a quartz glass body obtainable by this process. Furthermore,the invention relates to a light guide, an illuminant, and a formedbody, each of which is obtainable by further processing of the quartzglass body.

BACKGROUND OF THE INVENTION

Quartz glass, quartz glass products and products which contain quartzglass are known. Likewise, various processes for the preparation ofquartz glass and quartz glass bodies are already known. Nonetheless,considerable efforts are still being made to identify preparationprocesses by which quartz glass of even higher purity, i.e. absence ofimpurities, can be prepared. In many areas of application of quartzglass and its processed products, high demands are made, for example interms of homogeneity and purity. This is the case, inter alia, forquartz glass which is processed into light guides or illuminants. Here,impurities can cause absorptions. That is disadvantageous, since itleads to colour changes and attenuation of the emitted light. A furtherexample of an application of high purity quartz glass is productionsteps in the fabrication of semiconductors. Here, every impurity of theglass body can potentially lead to defects in the semiconductor and thusto rejects in the fabrication. The varieties of high purity quartz glasswhich are employed in these processes are laborious to prepare. Theseare valuable.

Furthermore, there is a market requirement for the above mentioned highpurity quartz glass and products derived therefrom at low price.Therefore, it is an aspiration to be able to offer high purity quartzglass at a lower price than before. In this connection, both morecost-efficient preparation processes as well as cheaper sources of rawmaterials are sought.

Known processes for the preparation of quartz glass bodies comprisemelting silicon dioxide and making quartz glass bodies out of the melt.Irregularities in a glass body, for example through inclusion of gasesin the form of bubbles, can lead to a failure of the glass body underload, in particular at high temperatures, or can preclude its use for aparticular purpose. Impurities in the raw materials for the quartz glasscan lead to cracks, bubbles, streaks and discolorations in the quartzglass. When employed in processes for the preparation and processing ofsemi-conductors, impurities in the glass body can also be released andtransferred to the treated semi-conductor components. This is the case,for example, in etching processes and leads to rejects in thesemi-conductor billets. A common problem associated with knownpreparation processes is therefore an inadequate quality of quartz glassbodies.

A further aspect relates to raw materials efficiency. It appearsadvantageous to input quartz glass and raw materials, which accumulateelsewhere as side products, into a preferably industrial process forquartz glass products, rather than employ these side products as filler,e.g. in construction or to dispose of them as rubbish at a cost. Theseside products are often separated off as fine dust in filters. The finedust brings further problems, in particular in relation to health, worksafety and handling.

Objects

An object of the present invention is to at least partially overcome oneor more of the disadvantages present in the state of the art.

It is a further object of the invention to provide light guides,illuminants and components with a long lifetime. The term components inparticular is to be understood to include devices which can be employedin reactors for chemical and/or physical treatment steps.

It is a further object of the invention to provide light guides,illuminants and glass components which are free of bubbles or have a lowcontent of bubbles.

It is a further object of the invention to provide light guides andglass components which have a high transparency.

It is a further object of the invention to provide light guides,illuminants and components which have a low opacity.

It is a further object of the invention to provide light guides with alow attenuation.

It is a further object of the invention to provide light guides,illuminants and components which have a high contour accuracy. Inparticular, it is an object of the invention to provide light guides,illuminants and components which do not deform at high temperatures. Inparticular, it is an object of the invention to provide light guides,illuminants and components which are form stable, even when formed withlarge size.

It is a further object of the invention to provide light guides,illuminants and components which are tear-proof and break-proof.

It is a further object of the invention to provide light guides,illuminants and components which are efficient to prepare.

It is a further object of the invention to provide light guides,illuminants and components which are cost-efficient to prepare.

It is a further object of the invention to provide light guides,illuminants and components, the preparation of which does not requirelong further processing steps, for example tempering.

It is a further object of the invention to provide light guides,illuminants and components which have a high thermal shock resistance.It is in particular an object of the invention to provide light guides,illuminants and components which with large thermal fluctuations exhibitonly little thermal expansion.

It is a further object of the invention to provide light guides,illuminants and components with a high hardness.

It is a further object of the invention to provide light guides,illuminants and components which have a high purity and lowcontamination with foreign atoms. The term foreign atoms is employed tomean constituents which are not purposefully introduced.

It is a further object of the invention to provide light guides,illuminants and components which contain a low content of dopantmaterials.

It is a further object of the invention to provide light guides,illuminants and components which have a high homogeneity. A homogeneityof a property or of a material is a measure of the uniformity of thedistribution of this property or material in a sample.

It is in particular an object of the invention to provide light guides,illuminants and components which have a high material homogeneity. Thematerial homogeneity is a measure of the uniformity of the distributionof the elements and compounds, in particularly of OH, chlorine, metals,in particular aluminium, alkali earth metals, refractory metals anddopant materials, contained in the light guide, illuminant orsemi-conductor device.

It is a further object of the invention to provide a quartz glass bodywhich is suitable for use in light guides, illuminants and quartz glasscomponents and solves at least partly at least one, preferably several,of the above mentioned objects.

It is a further object of the invention to provide a quartz glass bodywhich has a linear form. In particular, it is an object to provide aquartz glass body which has a high bending radius. In particular, it isa further object to provide a quartz glass body which has a high fibrecurl.

It is a further object to provide a quartz glass body in which themigration of cations is as low as possible.

It is a further object to provide a quartz glass body which has a highhomogeneity over the entire length of the quartz glass body.

In particular, it is a further object of the invention to provide aquartz glass body which has a high homogeneity of refractive index overthe entire length of the quartz glass body.

In particular, it is a further object of the invention to provide aquartz glass body which has a high homogeneity of viscosity over theentire length of the quartz glass body.

In particular, it is a further object of the invention to provide aquartz glass body which has a high material homogeneity over the entirelength of the quartz glass body.

In particular, it is a further object of the invention to provide aquartz glass body which has a high optical homogeneity over the entirelength of the quartz glass body.

It is a further object of the invention to provide a quartz glass bodywith a low OH content.

It is a further object to provide a quartz glass body which has a lowcontent of impurities from the crucible.

It is a further object of the invention to provide a silicon dioxidegranulate with a good handlability.

It is a further object of the invention to provide a silicon dioxidegranulate which has a low content of fine dust.

It is a further object to provide a silicon dioxide granulate which canbe easily stored, transported and conveyed.

It is a further object of the invention to provide a silicon dioxidegranulate which can form bubble free quartz glass bodies. It is afurther object of the invention to provide a silicon dioxide granulatewhich as a bulk material comprises as small a gas volume as possible.

It is a further object of the invention to provide an open-pored silicondioxide granulate.

It is a further object of the invention to provide a process by whichquartz glass bodies can be prepared by which at least part of the abovedescribed objects is at least partly solved.

It is a further object of the invention to provide a process by whichquartz glass bodies can be more simply prepared.

It is a further object of the invention to provide a process by whichquartz glass bodies can be prepared continuously.

It is a further object of the invention to provide a process by whichquartz glass bodies can be prepared by a continuous melting and formingprocess.

It is a further object of the invention to provide a process by whichquartz glass bodies can be formed with a high speed.

It is a further object of the invention to provide a process by whichquartz glass bodies can be prepared with a low reject rate.

It is a further object of the invention to provide a process by whichassemblable quartz glass bodies can be prepared.

It is a further object of the invention to provide an automated processby which quartz glass bodies can be prepared.

A further object is to provide a process by which a quartz glass bodycan be prepared as cheaply and quickly as possible.

In particular, it is an object of the invention to provide a process bywhich quartz glass bodies can be prepared wherein the system startuptimes are short.

A further object is to provide a process by which quartz glass bodiescan be made with low energy expenditure.

A further object is to provide a process by which quartz glass bodiescan be made avoiding particles entering them from the crucible.

It is a further object of the invention to provide a process with a highthroughput for the preparation of quartz glass bodies.

It is a further object of the invention to provide a process for thepreparation of quartz glass bodies which can handle high educt volumes.

It is a further object of the invention to provide a process for thepreparation of quartz glass bodies which can be conducted at hightemperatures.

It is a further object of the invention to provide a process for thepreparation of quartz glass bodies wherein a hygroscopic silicon dioxidegranulate can be processed without reducing the working life of thecrucible and without causing the crucible to corrode in particular.

It is a further object of the invention to provide a process for thepreparation of quartz glass bodies wherein a chlorinated silicon dioxidegranulate can be processed without reducing the working life of thecrucible, in particular without causing crucible corrosion.

It is a further object of the invention to provide a process for thepreparation of quartz glass bodies in which a silicon dioxide granulatecan be processed in a melting oven without the requirement for it to besubjected beforehand to a deliberate compacting step, e.g. by atemperature treatment of more than 1000° C.

It is in particular an object of the invention to provide a process forthe preparation of quartz glass bodies in which a silicon dioxidegranulate with a BET of 20 m²/g or more can be introduced into a meltingoven, melted and processed to obtain a quartz glass body.

It is a further object of the invention to provide a process for thepreparation of bubble-free quartz glass bodies by which open-poresilicon dioxide granulate can be processed.

A further object is to improve the processability of quartz glass bodiesfurther.

A further object is to improve the assemblability of quartz glass bodiesfurther.

Preferred Embodiments of the Invention

A contribution to at least partially fulfilling at least one of theaforementioned objects is made by the independent claims. The dependentclaims provide preferred embodiments which contribute to at leastpartially fulfilling at least one of the objects.

-   |1| A process for the preparation of a quartz glass body comprising    the process steps:    -   i.) Providing a silicon dioxide granulate        -   wherein the silicon dioxide granulate was made from            pyrogenic silicon dioxide powder and the silicon dioxide            granulate has the following feature;        -   A) a BET surface area in a range from 20 to 40 m²/g;    -   ii.) Making a glass melt out of the silicon dioxide granulate in        an oven;    -   iii.) Making a quartz glass body out of at least part of the        glass melt;    -   wherein the oven has at least a first and a further chamber        connected to one another by a passage,    -   wherein the first chamber and further chamber are at different        temperatures,    -   wherein the temperature in the first chamber is lower than the        temperature in the further chamber.-   |2| The process according to embodiment |1|, wherein there is an    additive in the first chamber selected from the group consisting of    halogen, inert gas, base, oxygen or a combination of two or more of    them.-   |3| The process according to embodiment |2|, wherein the halogen is    selected from the group consisting of chlorine, fluorine, compounds    containing chlorine, compounds containing fluorine and a combination    of two or more thereof and wherein the inert gas is selected from    the group consisting of nitrogen, helium and a combination of the    two.-   |4| The process according to one of the preceding embodiments,    wherein the pressure in the first chamber is less than 500 mbar.-   |5| The process according to one of the preceding embodiments,    -   wherein the silicon dioxide granulate has at least one of the        following features:    -   B) a mean particle size in a range from 50 to 500 μm;    -   C) a bulk density in a range from 0.5 to 1.2 g/cm³;    -   D) a carbon content of less than 10 ppm;    -   E) an aluminium content of less than 200 ppb;    -   F) a tamped density in a range from 0.7 to 1.2 g/cm³;    -   G) a pore volume in a range from 0.1 to 2.5 mL/g;    -   H) an angle of repose in a range from 23 to 26°;    -   I) a particle size distribution D₁₀ in a range from 50 to 150        μm;    -   J) a particle size distribution D₅₀ in a range from 150 to 300        μm;    -   K) a particle size distribution D₉₀ in a range from 250 to 620        μm,    -   wherein the ppm and ppb are each based on the total weight of        the silicon dioxide powder.-   |6| The process according to one of the preceding embodiments,    wherein the silicon dioxide is transported from the first to the    further chamber as granulate.-   |7| The process according to one of the preceding embodiments,    wherein the first chamber contains at least one element selected    from the group consisting of quartz glass, a refractory metal,    aluminium and a combination of two or more thereof-   |8| The process according to one of the preceding embodiments,    wherein the further chamber is a crucible of metal sheet or a sinter    material comprising a sinter metal, wherein the metal sheet or    sinter metal is selected from the group consisting of molybdenum,    tungsten and a combination thereof-   |9| The process according to one of the preceding embodiments,    wherein the BET surface area is not reduced to less than 5 m²/g    before step ii).

|10| The process according to one of the preceding embodiments, whereinthe melt energy is transmitted to the silicon dioxide granulate via asolid surface.

|11| The process according to one of the preceding embodiments, whereinhydrogen, helium, nitrogen or a combination of two or more of them ispresent in the gas space of the oven.

|12| The process according to one of the preceding embodiments, whereinproviding the silicon dioxide granulate comprises the following processsteps:

-   -   I. Providing silicon dioxide powder with the following        characteristics:        -   a. A BET surface area in a range from 20 to 60 m²/g, and        -   b. A bulk density in a range from 0.01 to 0.3 g/cm³;    -   II. Processing the silicon dioxide powder to obtain a silicon        dioxide granulate, wherein the silicon dioxide granulate has a        larger particle size than the silicon dioxide powder.

-   |13| The process according to embodiment |12|, wherein the silicon    dioxide powder in step I.

has at least one of the following features:

-   -   c. a carbon content of less than 50 ppm;    -   d. a chlorine content of less than 200 ppm;    -   e. an aluminium content of less than 200 ppb;    -   f. a total content of metals different to aluminium of less than        5 ppm;    -   g. at least 70 wt.-% of the powder particles have a primary        particle size in a range from 10 to 100 nm;    -   h. a tamped density in a range from 0.001 to 0.3 g/cm³;    -   i. a residual moisture content of less than 5 wt.-%;    -   j. a particle size distribution D₁₀ in a range from 1 to 7 μm;    -   k. a particle size distribution D₅₀ in a range from 6 to 15 μm;    -   1. a particle size distribution D₉₀ in a range from 10 to 40 μm;    -   wherein the wt.-%, ppm and ppb are each based on the total        weight of the silicon dioxide powder.

-   |14| The process according to one of the preceding embodiments,    wherein the silicon dioxide powder can be prepared from an element    selected from the group consisting of siloxanes, silicon alkoxides    and silicon halides.

-   |15| The process according to one of the preceding embodiments,    comprising the following process step:    -   iv) Forming a hollow body with at least one opening from the        quartz glass body.

-   |16| A quartz glass body obtainable by a process according to one of    the embodiments |1| to |15|.

-   |17| The quartz glass body according to embodiment |16|, having at    least one of the following features:    -   A] an OH content of less than 500 ppm;    -   B] a chlorine content of less than 60 ppm;    -   C] an aluminium content of less than 200 ppb;    -   D] an ODC content of less than 5·10¹⁵/cm³;    -   E] a metal content of metals different to aluminium of less than        1 ppm;    -   F] a viscosity (p=1013 hPa) in a range from log₁₀ (η(1250°        C.)/dPas)=11.4 to log₁₀ (q (1250° C.)/dPas)=12.9 or log₁₀        (η(1300° C.)/dPas)=11.1 to log₁₀ (η(1300° C.)/dPas)=12.2 or        log₁₀ (η(1350° C.)/dPas)=10.5 to log₁₀ (η(1350° C.)/dPas)=11.5;    -   G] a standard deviation of the OH content of not more than 10%,        based on the OH content A] of the quartz glass body;    -   H] a standard deviation of the Cl content of not more than 10%,        based on the Cl content B] of the quartz glass body;    -   I] a standard deviation of the Al content of not more than 10%,        based on the Al content C] of the quartz glass body;    -   J] a refractive index homogeneity of less than 10⁴;    -   K] a cylindrical form;    -   L] a tungsten content of less than 1000 ppb;    -   M] a molybdenum content of less than 1000 ppb,    -   wherein the ppb and ppm are each based on the total mass of the        quartz glass body.

-   |18| A process for the preparation of a light guide comprising the    following steps:    -   A/ Providing        -   A1/ a hollow body with at least one opening obtainable by a            process according to embodiment |15|, or        -   A2/ a quartz glass body according to one of the embodiments            |16| or |17|, wherein the quartz glass body is first            processed to obtain a hollow body with at least two            openings;    -   B/ Introducing one or multiple core rods into the quartz glass        body through the at least one opening to obtain a precursor;    -   C/ Drawing the precursor from step B/ in the warm to obtain the        light guide with one or several cores and a jacket M1.

-   |19| A process for the preparation of an illuminant comprising the    following steps:    -   (i) Providing        -   (i-1) a hollow body with at least one opening obtainable by            a process according to embodiment |15|; or        -   (i-2) a quartz glass body according to one of the            embodiments |16| or |17|, wherein the quartz glass body is            first processed to obtain a hollow body;    -   (ii) Optionally fitting the hollow body with electrodes;    -   (iii) Filling the hollow body with a gas.

-   |20| A process for the preparation of a formed body comprising the    following steps:    -   (1) Providing a quartz glass body according to one of the        embodiments |16| or |17|;    -   (2) Forming the quartz glass body to obtain the formed body.

-   |21| A use of an oven with at least two chambers with a    liquid-carrying connection between them for improving the purity,    transparency and homogeneity of quartz glass bodies, with a low OH    content at the same time and products which can be prepared from    them.

-   |22| A use of an oven with at least two chambers with a    liquid-carrying connection between them for the preparation of    products containing quartz glass selected from the group consisting    of a light guide, an illuminant and a formed body.

General

In the present description disclosed ranges also include the boundaryvalues. A disclosure of the form “in the range from X to Y” in relationto a parameter A therefore means that A can take the values X, Y andvalues in between X and Y. Ranges bounded on one side of the form “up toY” for a parameter A mean correspondingly the value Y and those lessthan Y.

DETAILED DESCRIPTION OF THE INVENTION

A first aspect of the present invention is a process for the preparationof a quartz glass body comprising the process steps:

-   -   i.) Providing a silicon dioxide granulate,        -   wherein the silicon dioxide granulate was prepared from            pyrogenic silicon dioxide powder and the silicon dioxide            granulate has the following feature:        -   A) A BET surface area in a range from 20 to 40 m²/g;    -   ii.) Making a glass melt out of the silicon dioxide granulate in        an oven;    -   iii.) Making a quartz glass body out of at least part of the        glass melt, wherein the oven has at least a first and a further        chamber connected to one another by a passage,        -   wherein the first and further chambers are at different            temperatures,        -   wherein the temperature in the first chamber is lower than            the temperature in the further chamber.

Step i.)

According to a preferred embodiment of the first aspect of theinvention, the provision of the silicon dioxide granulate comprises thefollowing process steps:

-   -   I. Providing a silicon dioxide powder; and    -   II. Processing the silicon dioxide powder to obtain a silicon        dioxide granulate, wherein the silicon dioxide granulate has a        greater particle diameter than the silicon dioxide powder.        -   wherein in the processing, preferably a silicon dioxide            granulate is formed with granules which have a spherical            morphology; wherein the processing is further preferably            effected by spray granulat or roll granulation.

A powder means particles of a dry solid material with a primary particlesize in the range from 1 to less than 100 nm.

The silicon dioxide granulate can be obtained by granulating silicondioxide powder. A silicon dioxide granulate commonly has a BET surfacearea of 3 m²/g or more and a density of less than 1.5 g/cm³. Granulatingmeans transforming powder particles into granules. During granulation,clusters of multiple silicon dioxide powder particles, i.e. largeragglomerates, form which are referred to as “silicon dioxide granules”.These are often also called “silicon dioxide granulate particles” or“granulate particles”. Collectively, the granules form a granulate, e.g.the silicon dioxide granules form a “silicon dioxide granulate”. Thesilicon dioxide granulate has a larger particle diameter than thesilicon dioxide powder.

The granulation procedure, for transforming a powder into a granulate,will be described in more detail later.

Silicon dioxide grain in the present context means silicon dioxideparticles which are obtainable by reduction in size of a silicon dioxidebody, in particular of a quartz glass body. A silicon dioxide graincommonly has a density of more than 1.2 g/cm³, for example in a rangefrom 1.2 to 2.2 g/cm³, and particularly preferably of about 2.2 g/cm³.Furthermore, the BET surface area of a silicon dioxide grain ispreferably generally less than 1 m²/g, determined according to DIN ISO9277:2014-01.

In principle, all silicon dioxide particles which are considered to besuitable by the skilled man can be selected. Preferred are silicondioxide granulate and silicon dioxide grain.

Particle diameter or particle size mean the diameter of a particle,given as the “area equivalent circular diameter x_(Ai)” according to theformula

${x_{Ai} = \sqrt{\frac{4A_{i}}{\pi}}},$

wherein Ai stands for the surface area of the observed particle by meansof image analysis. Suitable methods for the measurement are for exampleISO 13322-1:2014 or ISO 13322-2:2009. Comparative disclosures such as“greater particle diameter” always means that the values being comparedare measured with the same method.

Silicon Dioxide Powder

In the context of the present invention, pyrogenically produced silicondioxide powder is used.

The silicon dioxide powder can be any silicon dioxide powder which hasat least two particles. As preparation process, any process which theskilled man considers to be prevalent in the art and suitable can beused.

According to a preferred embodiment of the present invention, thesilicon dioxide powder is produced as side product in the preparation ofquartz glass, in particular in the preparation of so called “sootbodies”. Silicon dioxide from such a source is often also called “sootdust”.

A preferred source for the silicon dioxide powder are silicon dioxideparticles which are obtained from the synthetic preparation of sootbodies by application of flame hydrolysis burners. In the preparation ofa soot body, a rotating carrier tube with a cylinder jacket surface ismoved back and forth along a row of burners. Flame hydrolysis burnerscan be fed with oxygen and hydrogen as burner gases as well as the rawmaterials for making silicon dioxide primary particles. The silicondioxide primary particles preferably have a primary particle size of upto 100 nm. The silicon dioxide primary particles produced by flamehydrolysis aggregate or agglomerate to form silicon dioxide particleswith particle sizes of about 9 μm (DIN ISO 13320:2009-1). In the silicondioxide particles, the silicon dioxide primary particles areidentifiable by their form by scanning electron microscopy and theprimary particle size can be measured. A portion of the silicon dioxideparticles are deposited on the cylinder jacket surface of the carriertube which is rotating about its longitudinal axis. In this way, thesoot body is built up layer by layer. Another portion of the silicondioxide particles are not deposited on the cylinder jacket surface ofthe carrier tube, rather they accumulate as dust, e.g. in a filtersystem. This other portion of silicon dioxide particles make up thesilicon dioxide powder, often also called “soot dust”. In general, theportion of the silicon dioxide particles which are deposited on thecarrier tube is greater than the portion of silicon dioxide particleswhich accumulate as soot dust in the context of soot body preparation,based on the total weight of the silicon dioxide particles.

These days, soot dust is generally disposed of as waste in an onerousand costly manner, or used as filler material without adding value, e.g.in road construction, as additive in the dyes industry, as a rawmaterial for the tiling industry and for the preparation ofhexafluorosilicic acid, which is employed for restoration ofconstruction foundations. In the case of the present invention, it is asuitable raw material and can be processed to obtain a high-qualityproduct.

Silicon dioxide prepared by flame hydrolysis is normally calledpyrogenic silicon dioxide. Pyrogenic silicon dioxide is normallyavailable in the form of amorphous silicon dioxide primary particles orsilicon dioxide particles.

According to a preferred embodiment, the silicon dioxide powder can beprepared by flame hydrolysis out of a gas mixture. In this case, silicondioxide particles are also created in the flame hydrolysis and are takenaway before agglomerates or aggregates form. Here, the silicon dioxidepowder, previously referred to as soot dust, is the main product.

Suitable raw materials for creating the silicon dioxide powder arepreferably siloxanes, silicon alkoxides and inorganic silicon compounds.Siloxanes means linear and cyclic polyalkylsiloxanes. Preferably,polyalkylsiloxanes have the general formula

Si_(p)O_(p)R_(2p),

-   -   wherein p is an integer of at least 2, preferably from 2 to 10,        particularly preferably from 3 to 5, and    -   R is an alkyl group with 1 to 8 C-atoms, preferably with 1 to 4        C-atoms, particularly preferably a methyl group.

Particularly preferred are siloxanes selected from the group consistingof hexamethyldisiloxane, hexamethylcyclotrisiloxane (D3),octamethylcyclotetrasiloxane (D4) and decamethylcyclopentasiloxane (D5)or a combination of two or more thereof. If the siloxane comprises D3,D4 and D5, then D4 is preferably the main component. The main componentis preferably present in an amount of at least 70 wt.-%, preferably ofat least 80 wt.-%, for example of at least 90 wt.-% or of at least 94wt.-%, particularly preferably of at least 98 wt.-%, in each case basedon the total amount of the silicon dioxide powder. Preferred siliconalkoxides are tetramethoxysilane and methyltrimethoxysilane. Preferredinorganic silicon compounds as raw material for silicon dioxide powderare silicon halides, silicates, silicon carbide and silicon nitride.Particularly preferred inorganic silicon compounds as raw material forsilicon dioxide powder are silicon tetrachloride and trichlorosilane.

According to a preferred embodiment, the silicon dioxide powder can beprepared from a compound selected from the group consisting ofsiloxanes, silicon alkoxides and silicon halides.

Preferably, the silicon dioxide powder can be prepared from a compoundselected from the group consisting of hexamethyldisiloxane,hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane,decamethylcyclopentasiloxane, tetramethoxysilane,methyltrimethoxysilane, silicon tetrachloride and trichlorosilane or acombination of two or more thereof, for example out of silicontetrachloride and octamethylcyclotetrasiloxane, particularly preferablyout of octamethylcyclotetrasiloxane.

For making silicon dioxide out of silicon tetrachloride by flamehydrolysis, various parameters are significant. A preferred compositionof a suitable gas mixture comprises an oxygen content in the flamehydrolysis in a range from 25 to 40 vol.-%. The content of hydrogen canbe in a range from 45 to 60 vol.-%. The content of silicon tetrachlorideis preferably 5 to 30 vol.-%, all of the afore mentioned vol.-% beingbased on the total volume of the gas flow. Further preferred is acombination of the above mentioned volume proportions for oxygen,hydrogen and SiCl₄. The flame in the flame hydrolysis preferably has atemperature in a range from 1500 to 2500° C., for example in a rangefrom 1600 to 2400° C., particularly preferably in a range from 1700 to2300° C. Preferably, the silicon dioxide primary particles created inthe flame hydrolysis are taken away as silicon dioxide powder beforeagglomerates or aggregates form.

According to a preferred embodiment of the first aspect of theinvention, the silicon dioxide powder has the following features:

-   -   a. a BET surface area in a range from 20 to 60 m²/g, for example        from 25 to 55 m²/g, or from 30 to 50 m²/g, particularly        preferably from 20 to 40 m²/g, and    -   b. a bulk density 0.01 to 0.3 g/cm³, for example in the range        from 0.02 to 0.2 g/cm³, preferably in the range from 0.03 to        0.15 g/cm³, further preferably in the range from 0.1 to 0.2        g/cm³ or in the range from 0.05 to 0.1 g/cm³.

The silicon dioxide powder preferably has at least one, for example atleast two or at least three or at least four, particularly preferably atleast five of the following features:

-   -   c. a carbon content of less than 50 ppm, for example of less        than 40 ppm or of less than 30 ppm, particularly preferably in a        range from 1 ppb to 20 ppm;    -   d. a chlorine content of less than 200 ppm, for example of less        than 150 ppm or of less than 100 ppm, particularly preferably in        a range from 1 ppb to 80 ppm;    -   e. an aluminium content of less than 200 ppb, for example in the        range from 1 to 100 ppb, particularly preferably in the range        from 1 to 80 ppb;    -   f. a total content of metals different to aluminium of less than        5 ppm, for example of less than 2 ppm, particularly preferably        in a range from 1 ppb to 1 ppm;    -   g. at least 70 wt.-% of the powder particles have a primary        particle size in a range from 10 to less than 100 nm, for        example in the range from 15 to less than 100 nm, particularly        preferably in the range from 20 to less than 100 nm;    -   h. a tamped density in a range from 0.001 to 0.3 g/cm³, for        example in the range from 0.002 to 0.2 g/cm³ or from 0.005 to        0.1 g/cm³, preferably in the range from 0.01 to 0.06 g/cm³, and        preferably in the range from 0.1 to 0.2 g/cm³, or in the range        of from 0.15 to 0.2 g/cm³;    -   i. a residual moisture content of less than 5 wt.-%, for example        in the range from 0.25 to 3 wt.-%, particularly preferably in        the range from 0.5 to 2 wt.-%;    -   j. a particle size distribution D₁₀ in the range from 1 to 7 μm,        for example in the range from 2 to 6 μm or in the range from 3        to 5 μm, particularly preferably in the range from 3.5 to 4.5        μm;    -   k. a particle size distribution D₅₀ in the range from 6 to 15        μm, for example in the range from 7 to 13 μm or in the range        from 8 to 11 μm, particularly preferably in the range from 8.5        to 10.5 μm;    -   l. a particle size distribution D₉₀ in the range from 10 to 40        μm, for example in the range from 15 to 35 μm, particularly        preferably in the range from 20 to 30 μm;    -   wherein the wt.-%, ppm and ppb are each based on the total        weight of the silicon dioxide powder.

The silicon dioxide powder contains silicon dioxide. Preferably, thesilicon dioxide powder contains a proportion of silicon dioxide of morethan 95 wt.-%, for example more than 98 wt.-% or more than 99 wt.-%. ormore than 99.9 wt.-%, in each case based on the total weight of thesilicon dioxide powder. Particularly preferably, the silicon dioxidepowder contains a proportion of silicon dioxide of more than 99.99wt.-%, based on the total weight of the silicon dioxide powder.

Preferably, the silicon dioxide powder has a metal content of metalsdifferent from aluminium of less than 5 ppm, for example of less than 2ppm, particularly preferably of less than 1 ppm, in each case based onthe total weight of the silicon dioxide powder. Often however, thesilicon dioxide powder has a content of metals different to aluminium ofat least 1 ppb. Such metals are for example sodium, lithium, potassium,magnesium, calcium, strontium, germanium, copper, molybdenum, tungsten,titanium, iron and chromium. These can be present for example inelemental form, as an ion, or as part of a molecule or of an ion or of acomplex.

Preferably, the silicon dioxide powder has a total content of furtherconstituents of less than 30 ppm, for example of less than 20 ppm,particularly preferably of less than 15 ppm, the ppm in each case beingbased on the total weight of the silicon dioxide powder. Often however,the silicon dioxide powder has a content of further constituents of atleast 1 ppb. Further constituents means all constituents of the silicondioxide powder which do not belong to the following group: silicondioxide, chlorine, aluminium, OH-groups.

In the present context, reference to a constituent, when the constituentis a chemical element, means that it can be present as element or as anion or in a compound or a salt. For example the term “aluminium”includes in addition to metallic aluminium, also aluminium salts,aluminium oxides and aluminium metal complexes. For example, the term“chlorine” includes, in addition to elemental chlorine, chlorides suchas sodium chloride and hydrogen chloride. Often, the furtherconstituents are present in the same aggregate state as the material inwhich they are contained.

In the present context, in the case where a constituent is a chemicalcompound or a functional group, reference to the constituent means thatthe constituent can be present in the form disclosed, as a chargedchemical compound or as derivative of the chemical compound. Forexample, reference to the chemical material ethanol includes, inaddition to ethanol, also ethanolate, for example sodium ethanolate.Reference to “OH-group” also includes silanol, water and metalhydroxides. For example, reference to derivate in the context of aceticacid also includes acetic acid ester and acetic acid anhydride.

Preferably, at least 70% of the powder particles of the silicon dioxidepowder, based on the number of powder particles, have a primary particlesize of less than 100 nm, for example in the range from 10 to 100 nm orfrom 15 to 100 nm, and particularly preferably in the range from 20 to100 nm. The primary particle size is measured by dynamic lightscattering according to ISO 13320:2009-10.

Preferably at least 75% of the powder particles of the silicon dioxidepowder, based on the number of powder particles, have a primary particlesize of less than 100 nm, for example in the range from 10 to 100 nm orfrom 15 to 100 nm, and particularly preferably in the range from 20 to100 nm.

Preferably, at least 80% of the powder particles of the silicon dioxidepowder, based on the number of powder particles, have a primary particlesize of less than 100 nm, for example in the range from 10 to 100 nm orfrom 15 to 100 nm, and particularly preferably in the range from 20 to100 nm.

Preferably, at least 85% of the powder particles of the silicon dioxidepowder, based on the number of powder particles, have a primary particlesize of less than 100 nm, for example in the range from 10 to 100 nm orfrom 15 to 100 nm, and particularly preferably in the range from 20 to100 nm.

Preferably, at least 90% of the powder particles of the silicon dioxidepowder, based on the number of powder particles, have a primary particlesize of less than 100 nm, for example in the range from 10 to 100 nm orfrom 15 to 100 nm, and particularly preferably in the range from 20 to100 nm.

Preferably, at least 95% of the powder particles of the silicon dioxidepowder, based on the number of powder particles, have a primary particlesize of less than 100 nm, for example in the range from 10 to 100 nm orfrom 15 to 100 nm, and particularly preferably in the range from 20 to100 nm.

Preferably, the silicon dioxide powder has a particle size D₁₀ in therange from 1 to 7 μm, for example in the range from 2 to 6 μm or in therange from 3 to 5 μm, particularly preferably in the range from 3.5 to4.5 μm. Preferably, the silicon dioxide powder has a particle size D₅₀in the range from 6 to 15 μm, for example in the range from 7 to 13 μmor in the range from 8 to 11 μm, particularly preferably in the rangefrom 8.5 to 10.5 μm. Preferably, the silicon dioxide powder has aparticle size D90 in the range from 10 to 40 μm, for example in therange from 15 to 35 μm, particularly preferably in the range from 20 to30 μm.

Preferably, the silicon dioxide powder has a specific surface area(BET-surface area) in a range from 20 to 60 m²/g, for example from 25 to55 m²/g, or from 30 to 50 m²/g, particularly preferably from 20 to 40m²/g. The BET surface area is determined according to the method ofBrunauer, Emmet and Teller (BET) by means of DIN 66132 which is based ongas absorption at the surface to be measured.

Preferably, the silicon dioxide powder has a pH value of less than 7,for example in the range from 3 to 6.5 or from 3.5 to 6 or from 4 to5.5, particularly preferably in the range from 4.5 to 5. The pH valuecan be determined by means of a single rod measuring electrode (4%silicon dioxide powder in water).

The silicon dioxide powder preferably has the feature combinationa./b./c. or a./b./f. or a./b./g., further preferred the featurecombination a./b./c./f. or a./b./c./g. or a./b./f./g., furtherpreferably the feature combination a./b./c./f./g.

The silicon dioxide powder preferably has the feature combinationa./b./c., wherein the BET surface area is in a range from 20 to 40 m²/g,the bulk density is in a range from 0.05 to 0.3 g/mL and the carboncontent is less than 40 ppm.

The silicon dioxide powder preferably has the feature combinationa./b./f., wherein the BET surface area is in a range from 20 to 40 m²/g,the bulk density is in a range from 0.05 to 0.3 g/mL and the totalcontent of metals which are different to aluminium is in a range from 1ppb to 1 ppm.

The silicon dioxide powder preferably has the feature combinationa./b./g., wherein the BET surface area is in a range from 20 to 40 m²/g,the bulk density is in a range from 0.05 to 0.3 g/mL and at least 70 wt.% of the powder particles have a primary particle size in a range from20 to less than 100 nm.

The silicon dioxide powder further preferably has the featurecombination a./b./c./f., wherein the BET surface area is in a range from20 to 40 m²/g, the bulk density is in a range from 0.05 to 0.3 g/mL, thecarbon content is less than 40 ppm and the total content of metals whichare different to aluminium is in a range from 1 ppb to 1 ppm.

The silicon dioxide powder further preferably has the featurecombination a./b./c./g., wherein the BET surface area is in a range from20 to 40 m²/g, the bulk density is in a range from 0.05 to 0.3 g/mL, thecarbon content is less than 40 ppm and at least 70 wt. % of the powderparticles have a primary particle size in a range from 20 to less than100 nm.

The silicon dioxide powder further preferably has the featurecombination a./b./f./g., wherein the BET surface area is in a range from20 to 40 m²/g, the bulk density is in a range from 0.05 to 0.3 g/mL, thetotal content of metals which are different to aluminium is in a rangefrom 1 ppb to 1 ppm and at least 70 wt. % of the powder particles have aprimary particle size in a range from 20 to less than 100 nm.

The silicon dioxide powder has particularly preferably the featurecombination a./b./c./f./g., wherein the BET surface area is in a rangefrom 20 to 40 m²/g, the bulk density is in a range from 0.05 to 0.3g/mL, the carbon content is less than 40 ppm, the total content ofmetals which are different to aluminium is in a range from 1 ppb to 1ppm and at least 70 wt. % of the powder particles have a primaryparticle size in a range from 20 to less than 100 nm.

Step II.

According to a preferred embodiment of the first aspect of theinvention, silicon dioxide powder is processed in step II to obtain asilicon dioxide granulate, wherein the silicon dioxide granulate has agreater particle diameter than the silicon dioxide powder. For thispurpose, any processes known to the skilled man that lead to an increasein the particle diameter are suitable.

The silicon dioxide granulate has a particle diameter which is greaterthan the particle diameter of the silicon dioxide powder. Preferably,the particle diameter of the silicon dioxide granulate is in a rangefrom 500 to 50,000 times as great as the particle diameter of thesilicon dioxide powder, for example 1,000 to 10,000 times as great,particularly preferably 2,000 to 8,000 times as great.

Preferably, at least 90% of the silicon dioxide granulate provided instep i.) is made up of pyrogenically produced silicon dioxide powder,for example at least 95 wt.-% or at least 98 wt.-%, particularlypreferably at least 99 wt.-% or more, in each case based on the totalweight of the silicon dioxide granulate.

According to the invention, the silicon dioxide granulate employed hasthe following feature:

-   -   A) a BET surface area in the range from 20 m²/g to 40 m²/g.

The silicon dioxide granulate preferably has at least one, preferably atleast two or at least three or at least four, particularly preferablyall of the following features:

-   -   B) a mean particle size in a range from 50 to 500 μm.    -   C) a bulk density in a range from 0.5 to 1.2 g/cm³, for example        in a range from 0.6 to 1.1 g/cm³, particularly preferably in a        range from 0.7 to 1.0 g/cm³;    -   D) a carbon content of less than 50 ppm;    -   E) an aluminium content of less than 200 ppb;    -   F) a tamped density in a range from 0.7 to 1.2 g/cm³;    -   G) a pore volume in a range from 0.1 to 2.5 mL/g, for example in        a range from 0.15 to 1.5 mL/g; particularly preferably in a        range from 0.2 to 0.8 mL/g;    -   H) an angle of repose in a range from 23 to 26°;    -   I) a particle size distribution D₁₀ in a range from 50 to 150        μm;    -   J) a particle size distribution D₅₀ in a range from 150 to 300        μm;    -   K) a particle size distribution D₉₀ in a range from 250 to 620        μm,    -   wherein the ppm and ppb are each based on the total weight of        the silicon dioxide granulate.

Preferably, the granules of the silicon dioxide granulate have aspherical morphology. Spherical morphology means a round or oval form ofthe particle. The granules of the silicon dioxide granulate preferablyhave a mean sphericity in a range from 0.7 to 1.3 SPHT3, for example amean sphericity in a range from 0.8 to 1.2 SPHT3, particularlypreferably a mean sphericity in a range from 0.85 to 1.1 SPHT3. Thefeature SPHT3 is described in the test methods.

Furthermore, the granules of the silicon dioxide granulate preferablyhave a mean symmetry in a range from 0.7 to 1.3 Symm3, for example amean symmetry in a range from 0.8 to 1.2 Symm3, particularly preferablya mean symmetry in a range from 0.85 to 1.1 Symm3. The feature of themean symmetry Symm3 is described in the test methods.

Preferably, the silicon dioxide granulate has a metal content of metalsdifferent to aluminium of less than 1000 ppb, for example of less than500 ppb, particularly preferably of less than 100 ppb, in each casebased on the total weight of the silicon dioxide granulate. Oftenhowever, the silicon dioxide granulate has a content of metals differentto aluminium of at least 1 ppb. Often, the silicon dioxide granulate hasa metal content of metals different to aluminium of less than 1 ppm,preferably in a range from 40 to 900 ppb, for example in a range from 50to 700 ppb, particularly preferably in a range from 60 to 500 ppb, ineach case based on the total weight of the silicon dioxide granulate.Such metals are for example sodium, lithium, potassium, magnesium,calcium, strontium, germanium, copper, molybdenum, titanium, iron andchromium. These can for example be present as an element, as an ion, oras part of a molecule or of an ion or of a complex.

The silicon dioxide granulate can comprise further constituents, forexample in the form of molecules, ions or elements. Preferably, thesilicon dioxide granulate comprises less than 500 ppm of furtherconstituents, for example less than 300 ppm, particularly preferablyless than 100 ppm, in each case based on the total weight of the silicondioxide granulate. Often, at least 1 ppb of further constituents arecomprised. The further constituents can in particular be selected fromthe group consisting of carbon, fluoride, iodide, bromide, phosphorus ora mixture of at least two thereof.

Preferably, the silicon dioxide granulate comprises less than 10 ppmcarbon, for example less than 8 ppm or less than 5 ppm, particularlypreferably less than 4 ppm, in each case based on the total weight ofthe silicon dioxide granulate. Often, at least 1 ppb of carbon iscomprised in the silicon dioxide granulate.

Preferably, the silicon dioxide granulate comprises less than 100 ppm offurther constituents, for example less than 80 ppm, particularlypreferably less than 70 ppm, in each case based on the total weight ofthe silicon dioxide granulate. Often however, at least 1 ppb of thefurther constituents are comprised in the silicon dioxide granulate.

Preferably, step II. comprises the following steps:

-   -   II.1. Providing a liquid;    -   II.2. Mixing the silicon dioxide powder with the liquid to        obtain a slurry;    -   II.3. Granulating the slurry.

In the context of the present invention, a liquid means a material or amixture of materials which is liquid at a pressure of 1013 hPa and atemperature of 20° C.

A “slurry” in the context of the present invention means a mixture of atleast two materials, wherein the mixture, considered under theprevailing conditions, comprises at least one liquid and at least onesolid.

Suitable liquids are all materials and mixtures of materials known tothe skilled man and which appear suitable for the present application.Preferably, the liquid is selected from the group consisting of organicliquids and water. Preferably, the solubility of the silicon dioxidepowder in the liquid is less than 0.5 g/L, preferably less than 0.25g/L, particularly preferably less than 0.1 g/L, the g/L each given as gsilicon dioxide powder per litre liquid.

Preferred suitable liquids are polar solvents. These can be organicliquids or water. Preferably, the liquid is selected from the groupconsisting of water, methanol, ethanol, n-propanol, isopropanol,n-butanol, tert-butanol and mixtures of a more than one thereof.Particularly preferably, the liquid is water. Particularly preferably,the liquid comprises distilled or de-ionized water.

Preferably, the silicon dioxide powder is processed to obtain a slurry.The silicon dioxide powder is virtually insoluble in the liquid at roomtemperature, but can be introduced into the liquid in high weightproportions to obtain the slurry.

The silicon dioxide powder and the liquid can be mixed in any manner.For example, the silicon dioxide powder can be added to the liquid, orthe liquid can be added to the silicon dioxide powder. The mixture canbe agitated during the addition or following the addition. Particularlypreferably, the mixture is agitated during and following the addition.Examples for the agitation are shaking and stirring, or a combination ofboth. Preferably, the silicon dioxide powder can be added to the liquidunder stirring. Furthermore, preferably, a portion of the silicondioxide powder can be added to the liquid, wherein the mixture thusobtained is agitated, and the mixture is subsequently mixed with theremaining portion of the silicon dioxide powder. Likewise, a portion ofthe liquid can be added to the silicon dioxide powder, wherein themixture thus obtained is agitated, and the mixture subsequently mixedwith the remaining portion of the liquid.

By mixing the silicon dioxide powder and the liquid, a slurry isobtained. Preferably, the slurry is a suspension in which the silicondioxide powder is distributed uniformly in the liquid. “Uniform” meansthat the density and the composition of the slurry at each position doesnot deviate from the average density and from the average composition bymore than 10%, in each case based on the total amount of slurry. Auniform distribution of the silicon dioxide powder in the liquid canprepared, or obtained, or both, by an agitation as mentioned above.

Preferably, the slurry has a weight per litre in the range from 1000 to2000 g/L, for example in the range from 1200 to 1900 g/L or from 1300 to1800 g/L, particularly preferably in the range from 1400 to 1700 g/L.The weight per litre is measured by weighing a volume calibratedcontainer.

According to a preferred embodiment, at least one, for example at leasttwo or at least three or at least four, particularly preferably at leastfive of the following features applies to the slurry:

-   -   a.) the slurry is transported in contact with a plastic surface;    -   b.) the slurry is sheared;    -   c.) the slurry has a temperature of more than 0° C., preferably        in a range from 5 to 35° C.;    -   d.) the slurry has a zeta potential at a pH value of 7 in a        range from 0 to −100 mA, for example from −20 to −60 mA,        particularly preferably from −30 to −45 mA;    -   e.) the slurry has a pH value in a range of 7 or more, for        example of more than 7 or a pH value in the range from 7.5 to 13        or from 8 to 11, particularly preferably from 8.5 to 10;    -   f) the slurry has an isoelectric point of less than 7, for        example in a range from 1 to 5 or in a range from 2 to 4,        particularly preferably in a range from 3 to 3.5;    -   g.) the slurry has a solids content of at least 40 wt.-%, for        example in a range from 50 to 80 wt.-%, or in a range from 55 to        75 wt.-%, particularly preferably in a range from 60 to 70        wt.-%, in each case based on the total weight of the slurry;    -   h.) the slurry has a viscosity according to DIN 53019-1 (5 rpm,        30 wt.-%) in a range from 500 to 2000 mPas, for example in the        range from 600 to 1700 mPas, particularly preferably in the        range from 1000 to 1600 mPas;    -   i.) the slurry has a thixotropy according to DIN SPEC 91143-2        (30 wt.-% in water, 23° C., 5 rpm/50 rpm) in the range from 3 to        6, for example in the range from 3.5 to 5, particularly        preferably in the range from 4.0 to 4.5;    -   j.) the silicon dioxide particles in the slurry have in a 4        wt.-% slurry a mean particle size in suspension according to DIN        ISO 13320-1 in the range from 100 to 500 nm, for example in a        range from 200 to 300 nm.

Preferably, the silicon dioxide particles in a 4 wt.-% aqueous slurryhave a particle size D₁₀ in a range from 50 to 250 nm, particularlypreferably in the range from 100 to 150 nm. Preferably, the silicondioxide particles in a 4 wt.-% aqueous slurry have a particle size D₅₀in a range from 100 to 400 nm, particularly preferably in the range from200 to 250 nm. Preferably, the silicon dioxide particles in a 4 wt.-%aqueous slurry have a particle size D90 in a range from 200 to 600 nm,particularly preferably in a range from 350 to 400 nm. The particle sizeis measured according to DIN ISO 13320-1.

“Isoelectric point” means the pH value at which the zeta potential takesthe value 0. The zeta potential is measured according to ISO13099-2:2012.

Preferably, the pH value of the slurry is set to a value in the rangegiven above. Preferably, the pH value can be set by adding to the slurrymaterials such as NaOH or NH₃, for example as aqueous solution. Duringthis process, the slurry is often agitated.

Granulation

The silicon dioxide granulate is obtained from the silicon dioxidepowder by granulation. Granulation means the transformation of powderparticles into granules. During granulation, larger agglomerates whichare referred to as “silicon dioxide granules” are formed byagglomeration of multiple silicon dioxide powder particles. These areoften also called “silicon dioxide particles”, “silicon dioxidegranulate particles” or “granulate particles”. Collectively, granulesmake up a granulate, e.g. the silicon dioxide granules make up a“silicon dioxide granulate”.

In the present case, any granulation process which is known to theskilled man and appears to him to be suitable for the granulation ofsilicon dioxide powder can in principle be selected.

Granulation processes can be categorised as agglomeration granulationprocesses or press granulation processes, and further categorised as wetand dry granulation processes. Known methods are roll granulation in agranulation plate, spray granulation, centrifugal pulverisation,fluidised bed granulation, granulation processes employing a granulationmill, compactification, roll pressing, briquetting, scabbing orextruding.

Preferably, a silicon dioxide granulate is formed in the processingwhich has a spherical morphology; wherein the process is furtherpreferably performed by spray granulation or roll granulation. Furtherpreferably, a silicon dioxide granulate with granules having a sphericalmorphology comprises at most 50% of granules, preferably at most 40% ofgranules, further preferred at most 20% of granules, more preferablybetween 0 and 50%, between 0 and 40% or between 0 and 20%, or between 10and 50%, between 10 and 40% or between 10 and 20% of granules not havinga spherical morphology, the percentages in each case based on the totalnumber of granules in the granulate. The granules with a sphericalmorphology have the SPHT3 values described in the description.

Spray Drying

According to a preferred embodiment of the first aspect of theinvention, a silicon dioxide granulate is obtained by spray granulationof the slurry. Spray granulation is also known as spray drying.

Spray drying is preferably effected in a spray tower. For spray drying,the slurry is preferably put under pressure at a raised temperature. Thepressurised slurry is then depressurised via a nozzle and thus sprayedinto the spray tower. Subsequently, droplets form which instantly dryand first form dry minute particles (“nuclei”). The minute particlesform, together with a gas flow applied to the particles, a fluidisedbed. In this way, they are maintained in a floating state and can thusform a surface for drying further droplets.

The nozzle, through which the slurry is sprayed into the spray tower,preferably forms an inlet into the interior of the spray tower.

The nozzle preferably has a contact surface with the slurry duringspraying. “Contact surface” means the region of the nozzle which comesinto contact with the slurry during spraying. Often, at least part ofthe nozzle is formed as a tube through which the slurry is guided duringspraying, so that the inner side of the hollow tube comes into contactwith the slurry.

The contact surface preferably comprises a glass, a plastic or acombination thereof. Preferably, the contact surface comprises a glass,particularly preferably quartz glass. Preferably, the contact surfacecomprises a plastic. In principle, all plastics known to the skilledman, which are stable at the process temperatures and do not pass anyforeign atoms to the slurry, are suitable. Preferred plastics arepolyolefins, for example homo- or co-polymers comprising at least oneolefin, particularly preferably homo- or co-polymers comprisingpolypropylene, polyethylene, polybutadiene or combinations of two ormore thereof. Preferably, the contact surface is made of a glass, aplastic or a combination thereof, for example selected from the groupconsisting of quartz glass and polyolefins, particularly preferablyselected from the group consisting of quartz glass and homo- orco-polymers comprising polypropylene, polyethylene, polybutadiene orcombinations of two or more thereof. Preferably, the contact surfacecomprises no metals, in particular no tungsten, titanium, tantalum,chromium, cobalt, nickel, iron, vanadium, zirconium and manganese.

It is in principle possible for the contact surface and the furtherparts of the nozzle to be made of the same or from different materials.Preferably, the further parts of the nozzle comprise the same materialas the contact surface. It is likewise possible for the further parts ofthe nozzle to comprise a material different to the contact surface. Forexample, the contact surface can be coated with a suitable material, forexample with a glass or with a plastic.

Preferably, the nozzle is more than 70 wt.-%, based on the total weightof the nozzle, made out of an item selected from the group consisting ofglass, plastic or a combination of glass and plastic, for example morethan 75 wt.-% or more than 80 wt.-% or more than 85 wt.-% or more than90 wt.-% or more than 95 wt.-%, particularly preferably more than 99wt.-%.

Preferably, the nozzle comprises a nozzle plate. The nozzle plate ispreferably made of glass, plastic or a combination of glass and plastic.Preferably, the nozzle plate is made of glass, particularly preferablyquartz glass. Preferably, the nozzle plate is made of plastic. Preferredplastics are polyolefins, for example homo- or co-polymers comprising atleast one olefin, particularly preferably homo- or co-polymerscomprising polypropylene, polyethylene, polybutadiene or combinations oftwo or more thereof. Preferably, the nozzle plate comprises no metals,in particular no tungsten, titanium, tantalum, chromium, cobalt, nickel,iron, vanadium, zirconium and manganese.

Preferably, the nozzle comprises a screw twister. The screw twister ispreferably made of glass, plastic or a combination of glass and plastic.Preferably, the screw twister is made of glass, particularly preferablyquartz glass. Preferably, the screw twister is made of plastic.Preferred plastics are polyolefins, for example homo- or co-polymerscomprising at least one olefin, partitularly preferably homo- orco-polymers comprising polypropylene, polyethylene, polybutadiene orcombinations of two or more thereof. Preferably, the screw twistercomprises no metals, in particular no tungsten, titanium, tantalum,chromium, cobalt, nickel, iron, vanadium, zirconium and manganese.

Furthermore, the nozzle can comprise further constituents. Preferredfurther constituents are a nozzle body, particularly preferable is anozzle body which surrounds the screw twister and the nozzle plate, across piece and a baffle. Preferably, the nozzle comprises one or more,particularly preferably all, of the further constituents. The furtherconstituents can independently from each other be made of in principleany material which is known to the skilled man and which is suitable forthis purpose, for example of a metal comprising material, of glass or ofa plastic. Preferably, the nozzle body is made of glass, particularlypreferably quartz glass. Preferably, the further constituents are madeof plastic. Preferred plastics are polyolefins, for example homo- or toco-polymers comprising at least one olefin, particularly preferablyhomo- or co-polymers comprising polypropylene, polyethylene,polybutadiene or combinations of two or more thereof. Preferably, thefurther constituents comprise no metals, in particular no tungsten,titanium, tantalum, chromium, cobalt, nickel, iron, vanadium, zirconiumand manganese.

Preferably, the spray tower comprises a gas inlet and a gas outlet.Through the gas inlet, a gas can be introduced into the interior of thespray tower, and through the gas outlet it can be let out. It is alsopossible to introduce gas into the spray tower via the nozzle. Likewise,gas can be let out via the outlet of the spray tower. Furthermore, gascan preferably be introduced via the nozzle and a gas inlet of the spraytower, and let out via the outlet of the spray tower and a gas outlet ofthe spray tower.

Preferably, in the interior of the spray tower is present an atmosphereselected from air, an inert gas, at least two inert gases or acombination of air with at least one inert gas, preferably a combinationof air with at least one inert gas, and preferably two inert gases.Inert gasses are preferably selected from the list consisting ofnitrogen, helium, neon, argon, krypton and xenon. For example, in theinterior of the spray tower there is present air, nitrogen or Argon,particularly preferably air.

Further preferably, the atmosphere present in the spray tower is part ofa gas flow. The gas flow is preferably introduced into the spray towervia a gas inlet and let out via a gas outlet. It is also possible tointroduce parts of the gas flow via the nozzle and to let out parts ofthe gas flow via a solids outlet. The gas flow can take on furtherconstituents in the spray tower. These can come from the slurry duringthe spray drying and transfer to the gas flow.

Preferably, a dry gas flow is fed to the spray tower. A dry gas flowmeans a gas or a gas mixture which has a relative humidity at thetemperature set in the spray tower below the condensation point. Arelative air humidity of 100% corresponds to a water content of 17.5g/m³ at 20° C. The gas is preferably pre-warmed to a temperature in arange from 150 to 450° C., for example from 200 to 420° C. or from 300to 400° C., particularly preferably from 350 to 400° C.

The interior of the spray tower is preferably temperature-controllable.Preferably, the temperature in the interior of the spray tower has avalue up to 550° C., for example 300 to 500° C., particularly preferably350 to 450° C.

The gas flow preferably has a temperature at the gas inlet in a rangefrom 150 to 450° C., for example from 200 to 420° C. or from 300 to 400°C., particularly preferably from 350 to 400° C.

The gas flow which is let out at the solids outlet, at the gas outlet orat both locations, preferably has a temperature of less than 170° C.,for example from 50 to 150° C., particularly preferably from 100 to 130°C.

Furthermore, the difference between the temperature of the gas flow onintroduction and of the gas flow on expulsion is preferably in a rangefrom 100 to 330° C., for example from 150 to 300° C.

The thus obtained silicon dioxide granules are present as an agglomerateof individual particles of silicon dioxide powder. The individualparticles of the silicon dioxide powder continue to be recognizable inthe agglomerate. The mean particle size of the particles of the silicondioxide powder is preferably in the range from 10 to 1000 nm, forexample in the range from 20 to 500 nm or from 30 to 250 nm or from 35to 200 nm or from 40 to 150 nm, or particularly preferably in the rangefrom 50 to 100 nm. The mean particle size of these particles is measuredaccording to DIN ISO 13320-1.

The spray drying can be carried out in the presence of auxiliaries. Inprinciple, all materials can be employed as auxiliaries, which are knownto the skilled man and which appear suitable for the presentapplication. As auxiliary material for example, so-called binders can beconsidered.

Examples of suitable binding materials are metal oxides such as calciumoxide, metal carbonates such as calcium carbonate and polysaccharidessuch as cellulose, cellulose ether, starch and starch derivatives.

Particularly preferably, the spray drying is carried out in the contextof the present invention without auxiliaries.

Preferably, before, after or before and after the removal of the silicondioxide granulate from the spray tower a portion thereof is separatedoff. For separating off, all processes which are known to the skilledman and which appear suitable can be considered. Preferably, theseparating off is effected by a screening or a sieving.

Preferably, before removal from the spray tower of the silicon dioxidegranulate which have been formed by spray drying, particles with aparticle size of less than 50 μm, for example with a particle size ofless than 70 μm particularly preferably with a particle size of lessthan 90 μm are separated off by screening. The screening is effectedpreferably using a cyclone arrangement, which is preferably arranged inthe lower region of the spray tower, particularly preferably above theoutlet of the spray tower.

Preferably, after removal of the silicon dioxide granulate from thespray tower, particles with a particle size of greater than 1000 μm, forexample with a particle size of greater than 700 μm, particularlypreferably with a particle size of greater than 500 μm are separated offby sieving. The sieving of the particles can in principle be effected inaccordance with all processes known to the skilled man and which aresuitable for this purpose. Preferably, the sieving is effected using avibrating chute.

According to a preferred embodiment, the spray drying of the slurrythrough a nozzle into a spray tower is characterised by at least one,for example two or three, particularly preferably all of the followingfeatures:

-   -   a] spray granulation in a spray tower;    -   b] the presence of a pressure of the slurry at the nozzle of not        more than 40 bar, for example in a range from 1.3 to 20 bar,        from 1.5 to 18 bar or from 2 to 15 bar or from 4 to 13 bar, or        particularly preferably in the range from 5 to 12 bar, wherein        the pressure is given in absolute terms (relative to p=0 hPa);    -   c] a temperature of the droplets upon entering into the spray        tower in a range from 10 to 50° C., preferably in a range from        15 to 30° C., particularly preferably in a range from 18 to 25°        C.    -   d] a temperature at the side of the nozzle directed towards the        spray tower in a range from 100 to 450° C., for example in a        range from 250 to 440° C., particularly preferably from 350 to        430° C.;    -   e] A throughput of slurry through the nozzle in a range from        0.05 to 1 m³/h, for example in a range from 0.1 to 0.7 m³/h or        from 0.2 to 0.5 m³/h, particularly preferably in a range from        0.25 to 0.4 m³/h;    -   f] A solids content of the slurry of at least 40 wt.-%, for        example in a range from 50 to 80 wt.-%, or in a range from 55 to        75 wt.-%, particularly preferably in a range from 60 to 70        wt.-%, in each case based on the total weight of the slurry;    -   g] A gas inflow into the spray tower in a range from 10 to 100        kg/min, for example in a range from 20 to 80 kg/min or from 30        to 70 kg/min, particularly preferably in a range from 40 to 60        kg/min;    -   h] A temperature of the gas flow upon entering into the spray        tower in a range from 100 to 450° C., for example in a range        from 250 to 440° C., particularly preferably from 350 to 430°        C.;    -   i] A temperature of the gas flow at the exit out of the spray        tower of less than 170° C.;    -   j] The gas is selected from the group consisting of air,        nitrogen and helium, or a combination of two or more thereof;        preferably air;    -   k] a residual moisture content of the granulate on removal out        of the spray tower of less than 5 wt.-%, for example of less        than 3 wt.-% or of less than 1 wt.-% or in a range from 0.01 to        0.5 wt.-%, particularly preferably in a range from 0.1 to 0.3        wt.-%, in each case based on the total weight of the silicon        dioxide granulate created in the spray drying;    -   l] at least 50 wt.-% of the spray granulate, based on the total        weight of the silicon dioxide granulate created in the spray        drying, completes a flight time in a range from 1 to 100 s, for        example of a period from 10 to 80 s, particularly preferably        over a period from 25 to 70 s;    -   m] at least 50 wt.-% of the spray granulate, based on the total        weight of the silicon dioxide granulate created in the spray        drying, covers a flight path of more than 20 m, for example of        more than 30 or of more than 50 or of more than 70 or of more        than 100 or of more than 150 or of more than 200 or in a range        from 20 to 200 m or from 10 to 150 or from 20 to 100,        particularly preferably a range from 30 to 80 m.    -   n] the spray tower has a cylindrical geometry;    -   o] a height of the spray tower of more than 10 m, for example of        more than 15 m or of more than 20 m or of more than 25 m or of        more than 30 m or in a range from 10 to 25 m, particularly        preferably in a range from 15 to 20 m;    -   p] screening out of particles with a size of less than 90 μm        before the removal of the granulate from the spray tower;    -   q] sieving out of particles with a size of more than 500 μm        after the removal of the granulate from the spray tower,        preferably in a vibrating chute;    -   r] The exit of the droplets of the slurry out of the nozzle        occurs at an angle of 30 to 60 degrees from vertical,        particularly preferably at an angle of 45 degree from vertical.

Vertical means the direction of the gravitational force vector.

The flight path means the path covered by a droplet of slurry fromexiting out of the nozzle in the gas chamber of the spray tower to forma granule up to completion of the action of flying and falling. Theaction of flying and falling frequently ends by the granule impactingwith the floor of the spray tower impacting or the granule impactingwith other granules already lying on the floor of the spray tower,whichever occurs first.

The flight time is the period required by a granule to cover the flightpath in the spray tower. Preferably, the granules have a helical flightpath in the spray tower.

Preferably, at least 60 wt.-% of the spray granulate, based on the totalweight of the silicon dioxide granulate created in the spray drying,cover a mean flight path of more than 20 m, for example of more than 30or of more than 50 or of more than 70 or of more than 100 or of morethan 150 or of more than 200 or in a range from 20 to 200 m or from 10to 150 or from 20 to 100, particularly preferably a range from 30 to 80m.

Preferably, at least 70 wt.-% of the spray granulate, based on the totalweight of the silicon dioxide granulate created in the spray drying,cover a mean flight path of more than 20 m, for example of more than 30or of more than 50 or of more than 70 or of more than 100 or of morethan 150 or of more than 200 or in a range from 20 to 200 m or from 10to 150 or from 20 to 100, particularly preferably a range from 30 to 80m.

Preferably, at least 80 wt.-% of the spray granulate, based on the totalweight of the silicon dioxide granulate created in the spray drying,cover a mean flight path of more than 20 m, for example of more than 30or of more than 50 or of more than 70 or of more than 100 or of morethan 150 or of more than 200 or in a range from 20 to 200 m or from 10to 150 or from 20 to 100, particularly preferably a range from 30 to 80m.

Preferably, at least 90 wt.-% of the spray granulate, based on the totalweight of the silicon dioxide granulate created in the spray drying,cover a mean flight path of more than 20 m, for example of more than 30or of more than 50 or of more than 70 or of more than 100 or of morethan 150 or of more than 200 or in a range from 20 to 200 m or from 10to 150 or from 20 to 100, particularly preferably a range from 30 to 80m.

Roll Granulation

According to a preferred embodiment of the first aspect of the inventionof the invention, a silicon dioxide granulate is obtained by rollgranulation of the slurry.

The roll granulation is carried out by stirring the slurry in thepresence of a gas at raised temperature. Preferably, the rollgranulation is effected in a stirring vessel fitted with a stirringtool. Preferably, the stirring vessel rotates in the opposite sense tothe stirring tool. Preferably, the stirring vessel additionallycomprises an inlet through which the silicon dioxide powder can beintroduced into the stirring vessel, an outlet through which the silicondioxide granulate can be removed, a gas inlet and a gas outlet.

For stirring the slurry, preferably a pin-type stirring tool is used. Apin-type stirring tool means a stirring tool fitted with multipleelongate pins having their longitudinal axis coaxial with the rotationalaxis of the stirring tool. The trajectory of the pins preferably tracescoaxial circles around the axis of rotation.

Preferably, the slurry is set to a pH value of less than 7, for exampleto a pH value in the range from 2 to 6.5, particularly preferably to apH value in a range from 4 to 6. For setting the pH value, an inorganicacid is preferably used, for example an acid selected from the groupconsisting of hydrochloric acid, sulphuric acid, nitric acid andphosphoric acid, particularly preferably hydrochloric acid.

Preferably, in the stirring vessel is present an atmosphere selectedfrom air, an inert gas, at least two inert gases or a combination of airwith at least one inert gas, preferably at least two inert gases. Inertgases are preferably selected from the list consisting of nitrogen,helium, neon, argon, krypton and xenon. For example, air, nitrogen orargon is present in the stirring vessel, particularly preferably air.

Furthermore, preferably, the atmosphere present in the stirring vesselis part of a gas flow. The gas flow is preferably introduced into thestirring vessel via the gas inlet and let out via the gas outlet. Thegas flow can take on further constituents in the stirring vessel. Thesecan originate from the slurry in the roll granulation and transfer intothe gas flow.

Preferably, a dry gas flow is introduced to the stirring vessel. A drygas flow means a gas or a gas mixture which has a relative humidity atthe temperature set in the stirring vessel under the condensation point.The gas is preferably pre-warmed to a temperature in a range from 50 to300° C., for example from 80 to 250° C., particularly preferably from100 to 200° C.

Preferably, per 1 kg of the employed slurry, 10 to 150 m³ gas per houris introduced into the stirring vessel, for example 20 to 100 m³ gas perhour, particularly preferably 30 to 70 m³ gas per hour.

During the mixing, the slurry is dried by the gas flow to form silicondioxide granules. The granulate which is formed is removed from thestirring vessel.

Preferably, the removed granulate is dried further. Preferably, thedrying is effected continuously, for example in a rotary kiln. Preferredtemperatures for the drying are in a range from 80 to 250° C., forexample in a range from 100 to 200° C., particularly preferably in arange from 120 to 180° C.

In the context of the present invention, continuous in respect of aprocess means that it can be operated continuously. That means that theintroduction and removal of materials involved in the process can beeffected on an ongoing basis whilst the process is being run. It is notnecessary to interrupt the process for this.

Continuous as an attribute of an object, e.g. in relation to a“continuous oven”, means that this to object is configured in such a waythat a process carried out therein, or a process step carried outtherein, can be carried out continuously.

The granulate obtained from the roll granulation can be sieved. Thesieving occur before or after the drying. Preferably it is sieved beforedrying. Preferably, granules with a particle size of less than 50 μm,for example with a particle size of less than 80 μm, particularlypreferably with a particle size of less than 100 μm, are sieved out.Furthermore, preferably, granules with a particle size of greater than900 μm, for example with a particle size of greater than 700 μm,particularly preferably with a particle size of greater than 500 μm,sieved out. The sieving out of larger particles can in principle becarried out in accordance with any process known to the skilled man andwhich is suitable for this purpose. Preferably, the sieving out oflarger particles is carried out by means of a vibrating chute.

According to a preferred embodiment, the roll granulation ischaracterised by at least one, for example two or three, particularlypreferably all of the following features:

-   -   [a] The granulation is carried out in a rotating stirring        vessel;    -   [b] The granulation is carried out in a gas flow of 10 to 150 kg        gas per hour and per 1 kg slurry;    -   [c] The gas temperature on introduction is 40 to 200° C.;    -   [d] Granules with a particle size of less than 100 μm and of        more than 500 μm are sieved out;    -   [e] The granules formed have a residual moisture content of 15        to 30 wt.-%;    -   [f] The granules formed are dried at 80 to 250° C., preferably        in a continuous drying tube, particularly preferably to a        residual moisture content of less than 1 wt.-%.

Preferably, the silicon dioxide granules obtained by granulation,preferably by spray or roll granulation, also referred to as silicondioxide granulate I, is treated before it is processed to obtain quartzglass bodies. This pre-treatment can fulfil various purposes whicheither facilitate the processing to obtain quartz glass bodies orinfluence the properties of the resulting quartz glass body. Forexample, the silicon dioxide granulate I can be compactified, purified,surface-modified or dried.

Preferably, the silicon dioxide granulate I can by subjected to athermal, mechanical or chemical treatment or a combination of two ormore treatments, wherein a silicon dioxide granulate II is obtained.

Chemical

According to a preferred embodiment of the first aspect of theinvention, the silicon dioxide granulate I has a carbon contentw_(C(1)). The carbon content w_(C(1)) is preferably less than 50 ppm,for example in the range from less than 40 ppm or from less than 30 ppm,particularly preferably in a range from 1 ppb to 20 ppm, are each basedon the total weight of the silicon dioxide granulate I.

According to a preferred embodiment of the first aspect of theinvention, the silicon dioxide granulate I comprises at least twoparticles. Preferably, the at least two particles can carry out a motionrelative to each other. As means for bringing about the relative motion,in principle all means known to the skilled man and which appear to himto be suitable can be considered. Particular preferred is a mixing. Amixing can in principle be carried out in any manner. Preferably, afeed-oven is selected for this. Accordingly, the at least two particlescan preferably perform a motion relative to each other by being agitatedin a feed oven, for example in a rotary kiln.

Feed ovens mean ovens for which loading and unloading of the oven,so-called charging, is carried out continuously. Examples of feed-ovensare rotary kilns, roll-over type furnaces, belt conveyor ovens, conveyorovens, continuous pusher-type furnaces. Preferably, for treatment of thesilicon dioxide granulate I, rotary kilns are used.

According to a preferred embodiment of the first aspect of theinvention, the silicon dioxide granulate I is treated with a reactant toobtain a silicon dioxide granulate II. The treatment is carried out inorder to change the concentration of certain materials in the silicondioxide granulate. The silicon dioxide granulate I can have impuritiesor certain functionalities, the content of which should be reduced, suchas for example: OH groups, carbon containing compounds, transitionmetals, alkali metals and alkali earth metals. The impurities andfunctionalities can originate from the starting materials or can beintroduced in the course of the process. The treatment of the silicondioxide granulate I can serve various purposes. For example, employingtreated silicon dioxide granulate I, i.e. silicon dioxide granulate II,can simplify the processing of the silicon dioxide granulate to obtainquartz glass bodies. Furthermore, this selection can be employed to tunethe properties of the resulting quartz glass body. For example, thesilicon dioxide granulate I can be purified or surface modified. Thetreatment of the silicon dioxide granulate I can also be employed forimproving the properties of the resulting quartz glass bodies.

Preferably, a gas or a combination of multiple gases is suitable asreactant. This is also referred to as a gas mixture. In principle, allgases known to the skilled man can be employed, which are known for thespecified treatment and which appear to be suitable. Preferably, a gasselected from the group consisting of HCl, Cl₂, F₂, O₂, O₃, H₂, C₂F₄,C₂F₆, HClO₄, air, inert gas, e.g. N₂, He, Ne, Ar, Kr, or combinations oftwo or more thereof is employed. Preferably, the treatment is carriedout in the presence of a gas or a combination of two or more gases.Preferably, the treatment is carried out in a gas counter flow or a gasco-flow.

Preferably, the reactant is selected from the group consisting of HCl,Cl₂, F₂, O₂, O₃ or combinations of two or more thereof. Preferably,mixtures of two or more of the above-mentioned gases are used for thetreatment of silicon dioxide granulate I. Through the presence of F, Clor both, metals which are contained in silicon dioxide granulates I asimpurities, such as for example transition metals, alkali metals andalkali earth metals, can be removed. In this connection, the abovementioned metals can be converted along with constituents of the gasmixture under the process conditions to obtain gaseous compounds whichare subsequently drawn out and thus are no longer present in thegranulate. Furthermore, preferably, the OH content in the silicondioxide granulate I can be decreased by the treatment of the silicondioxide granulate I with these gases.

Preferably, a gas mixture of HCl and Cl₂ is employed as reactant.Preferably, the gas mixture has an HCl content in a range from 1 to 30vol.-%, for example in a range from 2 to 15 vol.-%, particularlypreferably in a range from 3 to 10 vol.-%. Likewise, the gas mixturepreferably has a Cl₂ content in a range from 20 to 70 vol.-%, forexample in a range from 25 to 65 vol.-%, particularly preferably in arange from 30 to 60 vol.-%. The remainder up to 100 vol.-% can be madeup of one or more inert gases, e.g. N₂, He, Ne, Ar, Kr, or of air.Preferably, the proportion of inert gas in the reactants is in a rangefrom 0 to less than 50 vol.-%, for example in a range from 1 to 40vol.-% or from 5 to 30 vol.-%, particularly preferably in a range from10 to 20 vol.%, in each case based on the total volume of the reactants.

O₂, C₂F₂, or mixtures thereof with Cl₂ are preferably used for purifyingsilicon dioxide granulate I which has been prepared from a siloxane orfrom a mixture of multiple siloxanes.

The reactant in the form of a gas or of a gas mixture is preferablycontacted with the silicon dioxide granulate as a gas flow or as part ofa gas flow with a throughput in a range from 50 to 2000 L/h, for examplein a range from 100 to 1000 L/h, particularly preferably in a range from200 to 500 L/h. A preferred embodiment of the contacting is a contact ofthe gas flow and silicon dioxide granulate in a feed oven, for examplein a rotary kiln. Another preferred embodiment of the contacting is afluidised bed process.

Through treatment of the silicon dioxide granulate I with the reactant,a silicon dioxide granulate II with a carbon content w_(C(2)) isobtained. The carbon content w_(C(2)) of the silicon dioxide granulateII is less than the carbon content w_(C(1)) of the silicon dioxidegranulate I, based on the total weight of the respective silicon dioxidegranulate. Preferably, w_(C(2)) is 0.5 to 99%, for example 20 to 80% or50 to 95%, particularly preferably 60 to 99% less than w_(C(1)).

Thermal

Preferably, the silicon dioxide granulate I is additionally subjected toa thermal or mechanical treatment or to a combination of thesetreatments. One or more of these additional treatments can be carriedout before or during the treatment with the reactant. Alternatively, oradditionally, the additional treatment can also be carried out on thesilicon dioxide granulate II. In what follows, the term “silicon dioxidegranulate” comprises the alternatives “silicon dioxide granulate I” and“silicon dioxide granulate II”. It is equally possible to carry out thetreatments described in the following to the “silicon dioxide granulateI”, or to the treated silicon dioxide granulate I, the “silicon dioxidegranulate II”.

The treatment of the silicon dioxide granulate can serve variouspurposes. For example, this treatment facilitates the processing of thesilicon dioxide granulate to obtain quartz glass bodies.

The treatment can also influence the properties of the resulting glassbody. For example, the silicon dioxide granulate can be compactified,purified, surface modified or dried. In this connection, the specificsurface area (BET) can decrease. Likewise, the bulk density and the meanparticle size can increase due to agglomerations of silicon dioxideparticles. The thermal treatment can be carried out dynamically orstatically.

For the dynamic thermal treatment, all ovens in which the silicondioxide granulate can be thermally treated whilst being agitated are inprinciple suitable. For the dynamic thermal treatment, preferably feedovens are used.

A preferred mean holding time of the silicon dioxide granulate in thedynamic thermal treatment is quantity dependent. Preferably, the meanholding time of the silicon dioxide granulate in the dynamic thermaltreatment is in the range from 10 to 180 min, for example in the rangefrom 20 to 120 min or from 30 to 90 min. Particularly preferably, themean holding time of the silicon dioxide granulate in the dynamicthermal treatment is in the range from 30 to 90 min.

In the case of a continuous process, a defined portion of the flow ofsilicon dioxide granulate is used as a sample load for the measurementof the holding time, e.g. a gram, a kilogram or a tonne. The start andend of the holding time are determined by the introduction into andexiting from the continuous oven operation.

Preferably, the throughput of the silicon dioxide granulate in acontinuous process for dynamic thermal treatment is in the range from 1to 50 kg/h, for example in the range from 5 to 40 kg/h or from 8 to 30kg/h. Particularly preferably, the throughput here is in the range from10 to 20 kg/h.

In the case of a discontinuous process for dynamic thermal treatment,the treatment time is given as the period of time between the loadingand subsequent unloading of the oven.

In the case of a discontinuous process for dynamic thermal treatment,the throughput is in a range from 1 to 50 kg/h, for example in the rangefrom 5 to 40 kg/h or from 8 to 30 kg/h. Particularly preferably, thethroughput is in the range from 10 to 20 kg/h. The throughput can beachieved using a sample load of a determined amount which is treated foran hour. According to another embodiment, the throughput can be achievedthrough a number of loads per hour, wherein the weight of a single loadcorresponds to the throughput per hour divided by the number of loads.In this event, time of treatment corresponds to the fraction of an hourwhich is given by 60 minutes divided by the number of loads per hour.

Preferably, the dynamic thermal treatment of the silicon dioxidegranulate is carried out at an oven temperature of at least 500° C., forexample in the range from 510 to 1700° C. or from 550 to 1500° C. orfrom 580 to 1300° C., particularly preferably in the range from 600 to1200° C.

Normally, the oven has the indicated temperature in the oven chamber.Preferably, this temperature deviates from the indicated temperature byless than 10% downwards or upwards, based on the entire treatment periodand the entire length of the oven as well as at every point in time inthe treatment as well as at every position in the oven.

Alternatively, in particular the continuous process of a dynamic thermaltreatment of the silicon dioxide granulate can by carried out atdiffering oven temperatures. For example, the oven can have a constanttemperature over the treatment period, wherein the temperature varies insection over the length of the oven. Such sections can be of the samelength or of different lengths. Preferably, in this case, thetemperature increases from the entrance of the oven to the exit of theoven. Preferably, the temperature at the entrance is at least 100° C.lower than at the exit, for example 150° C. lower or 200° C. lower or300° C. lower or 400° C. lower. Furthermore, preferably, the temperatureat the entrance is preferably at least 500° C., for example in the rangefrom 510 to 1700° C. or from 550 to 1500° C. or from 580 to 1300° C.,particularly preferably in the range from 600 to 1200° C. Furthermore,preferably, the temperature at the entrance is preferably at least 300°C., for example from 400 to 1000° C. or from 450 to 900° C. or from 500to 800° C. or from 550 to 750° C., particularly preferably from 600 to700° C. Furthermore, each of the temperature ranges given at the ovenentrance can be combined with each of the temperature ranges given atthe oven exit. Preferred combinations of oven entrance temperatureranges and oven exit temperature ranges are:

Oven entrance temperature Oven exit temperature range [° C.] range [°C.] 400-1000 510-1300 450-900 550-1260 480-850 580-1200 500-800 600-1100530-750 630-1050

For the static thermal treatment of the silicon dioxide granulatecrucibles arranged in an oven are preferably used. Suitable cruciblesare sinter crucibles or metal sheet crucibles. Preferred are rolledmetal sheet crucibles made out of multiple sheets which are rivetedtogether. Examples of crucible materials are refractory metals, inparticular tungsten, molybdenum and tantalum. The crucible canfurthermore be made of graphite or in the case of the crucible ofrefractory metals can be lined with graphite foil. Furthermore,preferably, the crucibles can be made of silicon dioxide. Particularlypreferably, silicon dioxide crucibles are employed.

The mean holding time of the silicon dioxide granulate in the staticthermal treatment is quantity dependent. Preferably, the mean holdingtime of the silicon dioxide granulate in the static thermal treatmentfor a 20 kg amount of silicon dioxide granulate I is in the range from10 to 180 min, for example in the range from 20 to 120 min, particularlypreferably in the range from 30 to 90 min.

Preferably, the static thermal treatment of the silicon dioxidegranulate is carried out at an oven temperature of at least 800° C., forexample in the range from 900 to 1700° C. or from 950 to 1600° C. orfrom 1000 to 1500° C. or from 1050 to 1400° C., particularly preferablyin the range from 1100 to 1300° C.

Preferably, the static thermal treatment of the silicon dioxidegranulate I is carried out at constant oven temperature. The staticthermal treatment can also be carried out at a varying oven temperature.Preferably, in this case, the temperature increases during thetreatment, wherein the temperature at the start of the treatment is atleast 50° C. lower than at the end, for example 70° C. lower or 80° C.lower or 100° C. lower or 110° C. lower, and wherein the temperature atthe end is preferably at least 800° C., for example in the range from900 to 1700° C. or from 950 to 1600° C. or from 1000 to 1500° C. or from1050 to 1400° C., particularly preferably in the range from 1100 to1300° C.

Mechanical

According to a further preferred embodiment, the silicon dioxidegranulate I can be mechanically treated. The mechanical treatment can becarried out for increasing the bulk density. The mechanical treatmentcan be combined with the above mentioned thermal treatment. A mechanicaltreatment can avoid the agglomerates in the silicon dioxide granulateand therefore the mean particle size of the individual, treated silicondioxide granules in the silicon dioxide granulate becoming too large. Anenlargement of the agglomerates can hinder the further processing orhave disadvantageous impacts on the properties of the quartz glassbodies prepared by the inventive process, or a combination of botheffects. A mechanical treatment of the silicon dioxide granulate alsopromotes a uniform contact of the surfaces of the individual silicondioxide granules with the gas or gases. This is in particular achievedby concurrent mechanical and chemical treatment with one or more gases.In this way, the effect of the chemical treatment can be improved.

The mechanical treatment of the silicon dioxide granulate can be carriedout by moving two or more silicon dioxide granules relative to eachother, for example by rotating the tube of a rotary kiln.

Preferably, the silicon dioxide granulate I is treated chemically,thermally and mechanically. Preferably, a simultaneous chemical, thermaland mechanical treatment of the silicon dioxide granulate I is carriedout.

In the chemical treatment, the content of impurities in the silicondioxide granulate I is reduced.

For this, the silicon dioxide granulate I can be treated in a rotarykiln at raised temperature and under a chlorine and oxygen containingatmosphere. Water present in the silicon dioxide granulate I evaporates,organic materials react to form CO and CO₂. Metal impurities can beconverted to volatile chlorine containing compounds.

Preferably, the silicon dioxide granulate I is treated in a chlorine andoxygen containing atmosphere in a rotary kiln at a temperature of atleast 500° C., preferably in a temperature range from 550 to 1300° C. orfrom 600 to 1260° C. or from 650 to 1200° C. or from 700 to 1000° C.,particularly preferably in a temperature range from 700 to 900° C. Thechlorine containing atmosphere contains for example HCl or Cl₂ or acombination of both. This treatment causes a reduction of the carboncontent.

Furthermore, preferably alkali and iron impurities are reduced.Preferably, a reduction of the number of OH groups is achieved. Attemperatures under 700° C., treatment periods can be long, attemperatures above 1100° C. there is a risk that pores of the granulateclose, trapping chlorine or gaseous chlorine compounds.

Preferably, it is also possible to carry out sequentially multiplechemical treatment steps, each concurrent with thermal and mechanicaltreatment. For example, the silicon dioxide granulate I can first betreated in a chlorine containing atmosphere and subsequently in anoxygen containing atmosphere. The low concentrations of carbon, hydroxylgroups and chlorine resulting therefrom facilitate the melting down ofthe silicon dioxide granulate II.

According to a further preferred embodiment, step II.2) is characterisedby at least one, for example by at least two or at least three,particularly preferably by a combination of all of the followingfeatures:

-   -   N1) The reactant comprises HCl, Cl₂ or a combination therefrom;    -   N2) The treatment is carried out in a rotary kiln;    -   N3) The treatment is carried out at a temperature in a range        from 600 to 900° C.;    -   N4) The reactant forms a counter flow;    -   N5) The reactant has a gas flow in a range from 50 to 2000 L/h,        preferably 100 to 1000 L/h, particularly preferably 200 to 500        L/h;    -   N6) The reactant has a volume proportion of inert gas in a range        from 0 to less than 50 vol.-%.

Preferably, the silicon dioxide granulate I has a particle diameterwhich is greater than the particle diameter of the silicon dioxidepowder. Preferably, the particle diameter of the silicon dioxidegranulate I is up to 300 times as great as the particle diameter of thesilicon dioxide powder, for example up to 250 times as great or up to200 times as great or up to 150 times as great or up to 100 times asgreat or up to 50 times as great or up to 20 times as great or up to 10times as great, particularly preferably 2 to 5 times as great.

The silicon dioxide granulate obtained in this way is also calledsilicon dioxide granulate II. Particularly preferably, the silicondioxide granulate II is obtained from the silicon dioxide granulate I ina rotary kiln by means of a combination of thermal, mechanical andchemical treatment.

The silicon dioxide granulate provided in step i.) is preferablyselected from the group consisting of silicon dioxide granulate I,silicon dioxide granulate II and a combination therefrom.

“Silicon dioxide granulate I” means a granulate of silicon dioxide whichis produced by granulation of silicon dioxide powder which was obtainedthrough pyrolysis of silicon compounds in a fuel gas flame. Preferredfuel gases are oxyhydrogen gas, natural gas or methane gas, particularlypreferable is oxyhydrogen gas.

“Silicon dioxide granulate II” means a granulate of silicon dioxidewhich is produced by post treatment of the silicon dioxide granulate I.Possible post treatments are chemical, thermal and/or mechanicaltreatments. This is described at length in the context of thedescription of the provision of the silicon dioxide granulate (processstep II. of the first aspect of the invention).

Particularly preferably, the silicon dioxide granulate provided in stepi.) is the silicon dioxide granulate I. The silicon dioxide granulate Ihas the following features:

-   -   [A] a BET surface area in the range from 20 to 50 m²/g, for        example in a range from 20 to 40 m²/g; particularly preferably        in a range from 25 to 35 m²/g; wherein the micro pore portion        preferably accounts for a BET surface area in a range from 4 to        5 m²/g; for example in a range from 4.1 to 4.9 m²/g;        particularly preferably in a range from 4.2 to 4.8 m²/g; and    -   [B] a mean particle size in a range from 180 to 300 μm.

Preferably, the silicon dioxide granulate I is characterised by at leastone, for example by at least two or at least three or at least four,particularly preferably by at least five of the following features:

-   -   [C] a bulk density in a range from 0.5 to 1.2 g/cm³, for example        in a range from 0.6 to 1.1 g/cm³, particularly preferably in a        range from 0.7 to 1.0 g/cm³;    -   [D] a carbon content of less than 50 ppm, for example less than        40 ppm or less than 30 ppm or less than 20 ppm or less than 10        ppm, particularly preferably in a range from 1 ppb to 5 ppm;    -   [E] an aluminium content of less than 200 ppb, preferably of        less than 100 ppb, for example of less than 50 ppb or from 1 to        200 ppb or from 15 to 100 ppb, particularly preferably in a        range from 1 to 50 ppb.    -   [F] a tamped density in a range from 0.5 to 1.2 g/cm³, for        example in a range from 0.6 to 1.1 g/cm³, particularly        preferably in a range from 0.75 to 1.0 g/cm³;    -   [G] a pore volume in a range from 0.1 to 1.5 mL/g, for example        in a range from 0.15 to 1.1 mL/g; particularly preferably in a        range from 0.2 to 0.8 mL/g,    -   [H] a chlorine content of less than 200 ppm, preferably of less        than 150 ppm, for example less than 100 ppm, or of less than 50        ppm, or of less than 1 ppm, or of less than 500 ppb, or of less        than 200 ppb, or in a range from 1 ppb to less than 200 ppm, or        from 1 ppb to 100 ppm, or from 1 ppb to 1 ppm, or from 10 ppb to        500 ppb, or from 10 ppb to 200 ppb, particularly preferably from        1 ppb to 80 ppb;    -   [I] metal content of metals which are different to aluminium of        less than 1000 ppb, preferably in a range from 1 to 900 ppb, for        example in a range from 1 to 700 ppb, particularly preferably in        a range from 1 to 500 ppb;    -   [J] a residual moisture content of less than 10 wt.-%,        preferably in a range from 0.01 wt.-% to 5 wt.-%, for example        from 0.02 to 1 wt.-%, particularly preferably from 0.03 to 0.5        wt.-%;    -   wherein the wt.-%, ppm and ppb are each based on the total        weight of the silicon dioxide granulate I.

The OH content, or hydroxyl group content, means the content of OHgroups in a material, for example in silicon dioxide powder, in silicondioxide granulate or in a quartz glass body. The content of OH groups ismeasured spectroscopically in the infrared by comparing the first andthe third OH bands.

The chlorine content means the content of elemental chlorine or chlorineions in the silicon dioxide granulate, in the silicon dioxide powder orin the quartz glass body.

The aluminium content means the content of elemental aluminium oraluminium ions in the silicon dioxide granulate, in the silicon dioxidepowder or in the quartz glass body.

Preferably, the silicon dioxide granulate I has a micro pore proportionin a range from 4 to 5 m²/g; for example in a range from 4.1 to 4.9m²/g; particularly preferably in a range from 4.2 to 4.8 m²/g.

The silicon dioxide granulate I preferably has a density in a range from2.1 to 2.3 g/cm³, particularly preferably in a range from 2.18 to 2.22g/cm³.

The silicon dioxide granulate I preferably has a mean particle size in arange from 180 to 300 μm, for example in a range from 220 to 280 μm,particularly preferably in a range from 230 to 270 μm.

The silicon dioxide granulate I preferably has a particle size D₅₀ in arange from 150 to 300 μm, for example in a range from 180 to 280 μm,particularly preferably in a range from 220 to 270 μm. Furthermore,preferably, the silicon dioxide granulate I has a particle size D₁₀ in arange from 50 to 150 μm, for example in a range from 80 to 150 μm,particularly preferably in a range from 100 to 150 μm. Furthermore,preferably, the silicon dioxide granulate I has a particle size D90 in arange from 250 to 620 μm, for example in a range from 280 to 550 μm,particularly preferably in a range from 300 to 450 μm.

The silicon dioxide granulate I preferably has the feature combination[A]/[B]/[C] or [A]/[B]/[E] or [A]/[B]/[G], further preferred the featurecombination [A]/[B]/[C]/[E] or [A]/[B]/[C]/[G] or [A]/[B]/[E]/[G],further preferably the feature combination [A]/[B]/[C]/[E]/[G].

The silicon dioxide granulate I preferably has the feature combination[A]/[B]/[C], wherein the BET surface area is in a range from 20 to 40m²/g, the mean particle size is in a range from 180 to 300 μm and thebulk density is in a range from 0.6 to 1.1 g/mL.

The silicon dioxide granulate I preferably has the feature combination[A]/[B]/[E], wherein the BET surface area is in a range from 20 to 40m²/g, the mean particle size is in a range from 180 to 300 μm and thealuminium content is in a range from 1 to 50 ppb.

The silicon dioxide granulate I preferably has the featurecombination[A]/[B]/[G], wherein the BET surface area is in a range from20 to 40 m²/g, the mean particle size is in a range from 180 to 300 μmand the pore volume is in a range from 0.2 to 0.8 mL/g.

The silicon dioxide granulate I preferably has the feature combination[A]/[B]/[C]/[E], wherein the BET surface area is in a range from 20 to40 m²/g, the mean particle size is in a range from 180 to 300 μm, thebulk density is in a range from 0.6 to 1.1 g/mL and the aluminiumcontent is in a range from 1 to 50 ppb.

The silicon dioxide granulate I preferably has the feature combination[A]/[B]/[C]/[G], wherein the BET surface area is in a range from 20 to40 m²/g, the mean particle size is in a range from 180 to 300 μm, thebulk density is in a range from 0.6 to 1.1 g/mL and the pore volume isin a range from 0.2 to 0.8 mL/g.

The silicon dioxide granulate I preferably has the feature combination[A]/[B]/[E]/[G], wherein the BET surface area is in a range from 20 to40 m²/g, the mean particle size is in a range from 180 to 300 μm, thealuminium content is in a range from 1 to 50 ppb and the pore volume isin a range from 0.2 to 0.8 mL/g.

The silicon dioxide granulate I preferably has the feature combination[A]/[B]/[C]/[E]/[G], wherein the BET surface area is in a range from 20to 40 m²/g, the mean particle size is in a range from 180 to 300 μm, thebulk density is in a range from 0.6 to 1.1 g/mL, the aluminium contentis in a range from 1 to 50 ppb and the pore volume is in a range from0.2 to 0.8 mL/g.

Particle size means the size of the particles of aggregated primaryparticles, which are present in a silicon dioxide powder, in a slurry orin a silicon dioxide granulate. The mean particle size means thearithmetic mean of all particle sizes of the indicated material. The D₅₀value indicates that 50% of the particles, based on the total number ofparticles, are smaller than the indicated value. The D₁₀ value indicatesthat 10% of the particles, based on the total number of particles, aresmaller than the indicated value. The D₉₀ value indicates that 90% ofthe particles, based on the total number of particles, are smaller thanthe indicated value. The particle size is measured by the dynamic photoanalysis process according to ISO 13322-2:2006-11.

Furthermore, particularly preferably, the silicon dioxide granulateprovided in step i.) is the silicon dioxide granulate II. The silicondioxide granulate II has the following features:

-   -   (A) a BET surface area in the range from 10 to 35 m²/g, for        example in a range from 10 to 30 m²/g, particularly preferably        in a range from 20 to 30 m²/g; and    -   (B) a mean particle size in a range from 100 to 300 μm, for        example in a range from 150 to 280 μm or from 200 to 270 μm,        particularly preferably in a range from 230 to 260 μm.

Preferably, the silicon dioxide granulate II has at least one, forexample at least two or at least three or at least four, particularlypreferably at least five of the following features:

-   -   (C) a bulk density in a range from 0.7 to 1.2 g/cm³, for example        in a range from 0.75 to 1.1 g/cm³, particularly preferably in a        range from 0.8 to 1.0 g/cm³;    -   (D) a carbon content of less than 5 ppm, for example less than        4.5 ppm or in a range from 1 ppb to 4 ppm, particularly        preferably of less than 4 ppm;    -   (E) an aluminium content of less than 200 ppb, for example of        less than 150 ppb or of less than 100 ppb or from 1 to 150 ppb        or from 1 to 100 ppb, particularly preferably in a range from 1        to 80 ppb;    -   (F) a tamped density in a range from 0.7 to 1.2 g/cm³, for        example in a range from 0.75 to 1.1 g/cm³, particularly        preferably in a range from 0.8 to 1.0 g/cm³;    -   (G) a pore volume in a range from 0.1 to 2.5 mL/g, for example        in a range from 0.2 to 1.5 mL/g; particularly preferably in a        range from 0.4 to 1 mL/g;    -   (H) a chlorine content of less than 500 ppm, preferably of less        than 400 ppm, for example less than 350 ppm or preferably of        less than 330 ppm or in a range from 1 ppb to 500 ppm or from 10        ppb to 450 ppm particularly preferably from 50 ppb to 300 ppm;    -   (I) a metal content of metals which are different to aluminium        of less than 1000 ppb, for example in a range from 1 to 400 ppb,        particularly preferably in a range from 1 to 200 ppb;    -   (J) a residual moisture content of less than 3 wt.-%, for        example in a range from 0.001 wt.-% to 2 wt.-%, particularly        preferably from 0.01 to 1 wt.-%,    -   wherein the wt.-%, ppm and ppb are each based on the total        weight of the silicon dioxide granulate II.

Preferably, the silicon dioxide granulate II has a micro pore proportionin a range from 1 to 2 m²/g, for example in a range from 1.2 to 1.9m²/g, particularly preferably in a range from 1.3 to 1.8 m²/g.

The silicon dioxide granulate II preferably has a density in a rangefrom 0.5 to 2.0 g/cm³, for example from 0.6 to 1.5 g/cm³, particularlypreferably from 0.8 to 1.2 g/cm³. The density is measured according tothe method described in the test methods.

The silicon dioxide granulate II preferably has a particle size D₅₀ in arange from 150 to 250 μm, for example in a range from 180 to 250 μm,particularly preferably in a range from 200 to 250 μm. Furthermore,preferably, the silicon dioxide granulate II has a particle size D₁₀ ina range from 50 to 150 μm, for example in a range from 80 to 150 μm,particularly preferably in a range from 100 to 150 μm. Furthermore,preferably, the silicon dioxide granulate II has a particle size D₉₀ ina range from 250 to 450 μm, for example in a range from 280 to 420 μm,particularly preferably in a range from 300 to 400 μm.

The silicon dioxide granulate II preferably has the feature combination(A)/(B)/(D) or (A)/(B)/(F) or (A)/(B)/(I), further preferred the featurecombination (A)/(B)/(D)/(F) or (A)/(B)/(D)/(I) or (A)/(B)/(F)/(I),further preferably the feature combination (A)/(B)/(D)/(F)/(I).

The silicon dioxide granulate II preferably has the feature combination(A)/(B)/(D), wherein the BET surface area is in a range from 10 to 30m²/g, the mean particle size is in a range from 150 to 280 μm and thecarbon content is less than 4 ppm.

The silicon dioxide granulate II preferably has the feature combination(A)/(B)/(F), wherein the BET surface area is in a range from 10 to 30m²/g, the mean particle size is in a range from 150 to 280 μm and Thetamped density is in a range from 0.8 to 1.0 g/mL.

The silicon dioxide granulate II preferably has the feature combination(A)/(B)/(I), wherein the BET surface area is in a range from 10 to 30m²/g, the mean particle size is in a range from 150 to 280 μm and themetal content of metals which are different to aluminium is in a rangefrom 1 to 400 ppb.

The silicon dioxide granulate II preferably has the feature combination(A)/(B)/(D)/(F), wherein the BET surface area is in a range from 10 to30 m²/g, the mean particle size is in a range from 150 to 280 μm, thecarbon content is less than 4 ppm and The tamped density is in a rangefrom 0.8 to 1.0 g/mL.

The silicon dioxide granulate II preferably has the feature combination(A)/(B)/(D)/(I), wherein the BET surface area is in a range from 10 to30 m²/g, the mean particle size is in a range from 150 to 280 μm, thecarbon content is less than 4 ppm and the metal content of metals whichare different to aluminium is in a range from 1 to 400 ppb.

The silicon dioxide granulate II preferably has the feature combination(A)/(B)/(F)/(I), wherein the BET surface area is in a range from 10 to30 m²/g, the mean particle size is in a range from 150 to 280 μm, Thetamped density is in a range from 0.8 to 1.0 g/mL and the metal contentof metals which are different to aluminium is in a range from 1 to 400ppb.

The silicon dioxide granulate II preferably has the feature combination(A)/(B)/(D)/(F)/(I), wherein the BET surface area is in a range from 10to 30 m²/g, the mean particle size is in a range from 150 to 280 μm, thecarbon content is less than 4 ppm, The tamped density is in a range from0.8 to 1.0 g/mL and the metal content of metals which are different toaluminium is in a range from 1 to 400 ppb.

Step ii.)

According to step ii.), a glass melt is formed out of the silicondioxide granulate. Normally, the silicon dioxide granulate is warmeduntil a glass melt is obtained. The warming of the silicon dioxidegranulate to obtain a glass melt can in principle by carried out by anyway known to the skilled man for this purpose.

V-Zug for the Preparation of a Glass Melt

The formation of a glass melt from the silicon dioxide granulate, forexample by warming, can be carried out by a continuous process. In theprocess according to the invention for the preparation of a quartz glassbody, the silicon dioxide granulate can preferably be introducedcontinuously into an oven or the glass melt can be removed continuouslyfrom the oven, or both. Particularly preferably, the silicon dioxidegranulate is introduced continuously into the oven and the glass melt isremoved continuously from the oven.

For this, an oven which has at least one inlet and at least one outletis in principle suitable. An inlet means an opening through whichsilicon dioxide and optionally further materials can be introduced intothe oven. An outlet means an opening through which at least a part ofthe silicon dioxide can be removed from the oven. The oven can forexample be arranged vertically or horizontally. Preferably, the oven isarranged vertically. Preferably, at least one inlet is located above atleast one outlet. “Above” in connection with fixtures and features of anoven means, in particular in connection with an inlet and outlet, thatthe fixture or the features which is arranged “above” another has ahigher position above the zero of absolute height. “Vertical” means thatthe line directly joining the inlet and the outlet of the oven deviatesnot more than 30° from the direction of gravity.

According to a preferred embodiment of the first aspect of theinvention, the oven comprises a hanging metal sheet crucible. Into thehanging metal sheet crucible is introduced the silicon dioxide granulateand warmed to obtain a glass melt. A metal sheet crucible means acrucible which comprises at least one rolled metal sheet. Preferably, ametal sheet crucible has multiple rolled metal sheets. A hanging metalsheet crucible means a metal sheet crucible as previously describedwhich is arranged in an oven in a hanging position.

The hanging metal sheet crucible can in principle be made of allmaterials which are known to the skilled man and which are suitable formelting silicon dioxide. Preferably, the metal sheet of the hangingmetal sheet crucible comprises a sintered material, for example a sintermetal. Sinter metals means metals or alloys which are obtained bysintering of metal powders.

Preferably, the metal sheet of the metal sheet crucible comprises atleast one item selected from the group consisting of the refractorymetals. Refractory metals means metals of group 4 (Ti, Zr, Hf), of group5 (V, Nb, Ta) and of group 6 (Cr, Mo, W).

Preferably, the metal sheet of the metal sheet crucible comprises asinter metal selected from the group consisting of molybdenum, tungstenor a combination thereof. Furthermore, preferably, the metal sheet ofthe metal sheet crucible comprises at least one further refractorymetal, particularly preferably rhenium, osmium, iridium, ruthenium or acombination of two or more thereof.

Preferably, the metal sheet of the metal sheet crucible comprises analloy of molybdenum with a refractory metal, or tungsten with arefractory metal. Particularly preferred alloy metals are rhenium,osmium, iridium, ruthenium or a combination of two or more thereof.According to a further example, the metal sheet of the metal sheetcrucible is an alloy of molybdenum with tungsten, rhenium, osmium,iridium, ruthenium or a combination of two or more thereof. For examplethe metal sheet of the metal sheet crucible can be an alloy of tungstenwith molybdenum, rhenium, osmium, iridium, ruthenium or a combination oftwo or more thereof.

Preferably, the above described metal sheet of the metal sheet cruciblecan be coated with a refractory metal. According to a preferred example,the metal sheet of the metal sheet crucible is coated with rhenium,osmium, iridium, ruthenium, molybdenum or tungsten, or a combination oftwo or more thereof.

Preferably, the metal sheet and the coating have different compositions.For example a molybdenum metal sheet can be coated with one or multiplecoats of rhenium, osmium, iridium, ruthenium, tungsten or a combinationof two or more thereof. According to another example, a tungsten metalsheet is coated with one or multiple layers of rhenium, osmium, iridium,ruthenium, molybdenum or a combination of two or more thereof. Accordingto a further example, the metal sheet of the metal sheet crucible can bemade of molybdenum alloyed with rhenium or of tungsten alloyed withrhenium, and be coated on the inner side of the crucible with one ormultiple layers comprising rhenium, osmium, iridium, ruthenium or acombination of two or more thereof.

Preferably, the metal sheet of the hanging metal sheet crucible has adensity 95% or greater of the theoretical density, for example from 95%to 98% or from 96% to 98%. More preferable are higher theoreticaldensities, in particular in the range from 98 to 99.95%. The theoreticaldensity of a basic material corresponds to the density of a pore freeand 100% dense material.

A density of the metal sheet of the metal sheet crucible of more than95% of the theoretical density can for example be obtained by sinteringa sinter metal and subsequent compactification of the sintered metal.Particularly preferably, a metal sheet crucible is obtainable bysintering of a sinter metal, rolling to obtain a metal sheet andprocessing the metal sheet to obtain a crucible.

Preferably, the metal sheet crucible has at least a lid, a wall and abase plate. Preferably, the hanging metal sheet crucible has at leastone, for example at least two or at least three or at least four,particularly preferably at least five or all of the following features:

-   -   (a) at least one, e.g. more than one or at least two or at least        three or at least five, particularly preferably three or four        layers of the metal sheet;    -   (b) at least one metal sheet, e.g. at least three or at least        four or at least six or at least eight or at least twelve or at        least 15 or at least 16 or at least 20 metal sheets,        particularly preferably twelve or 16 metal sheets;    -   (c) at least one join between two metal sheet parts, e.g. at        least two or at least five or at least ten or at least 18 or at        least 24 or at least 36 or at least 48 or at least 60 or at        least 72 or at least 48 or at least 96 or at least 120 or at        least 160, particularly preferably 36 or 48 joins between two of        the same or between multiple different metal sheet parts of the        hanging metal sheet crucible;    -   (d) The metal sheet parts of the hanging metal sheet crucible        are riveted, e.g. by deep drawing at least one joint e.g. joined        by a combination of deep drawing with metal sheet collaring or        countersinking, screwed or welded e.g. electron beam welding and        sintering of the weld points, the metal sheet parts are        particularly preferably riveted;    -   (e) The metal sheet of the hanging metal sheet crucible is        obtainable by a shaping step which is associated with an        increase of the physical density, preferably by shaping of a        sintered metal or of a sintered alloy; furthermore, preferably,        the shaping is a rolling;    -   (f) A hanger assembly of copper, aluminium, steel, iron, nickel        or a refractory metal, e.g. of the crucible material, preferably        a water cooled hanger assembly of copper or steel;    -   (g) A nozzle, preferably a nozzle permanently fixed to the        crucible;    -   (h) A mandrel, for example a mandrel fixed to the nozzle with        pins or a mandrel fixed to the lid with a supporting rod or a        mandrel attached underneath the crucible with a supporting rod;    -   (i) at least one gas inlet, e.g. in the form of a filling pipe        or as a separate inlet;    -   (j) at least one gas outlet, e.g. as a separate outlet in the        lid or in the wall of the crucible;    -   (k) a cooled jacket, preferably a water cooled jacket;    -   (l) an insulation on the outside, preferably an insulation on        the outside made of zirconium oxide.

The hanging metal sheet crucible can in principle be heated in any waywhich is known to the skilled person and which seems to him to besuitable. The hanging metal sheet crucible can for example be heated bymeans of electrical heating elements (resistive) or by induction. In thecase of resistive heating, the solid surface of the metal sheet crucibleis warmed from the outside and delivers the energy from there to itsinner side. For inductive heating, the energy is coupled directly intothe side wall of the melting crucible using coils and is transferredfrom there to the inner side of the crucible. For a resistive heating,the energy is coupled via radiation, whereby the solid surface is warmedfrom outside and the energy is transferred from there to the inside.Preferably, the melting crucible is heated inductively.

According to a preferred embodiment of the present invention, the energytransfer into the melting crucible, in particular for melting a bulkmaterial, is not performed by warming the melting crucible, or a bulkmaterial present therein, or both, using a flame, such as for example aburner flame directed into the melting crucible or onto the meltingcrucible.

By means of the hanging arrangement, the hanging metal sheet cruciblecan be moved in the oven. Preferably, the crucible can be at leastpartially moved into and moved out of the oven. If different heatingzones are present in the oven, their temperature profile will betransferred to the crucible which is present in the oven. By changingthe position of the crucible in the oven, multiple heating zones,varying heating zones or multiple varying heating zones can be producedin the crucible.

The metal sheet crucible has a nozzle. The nozzle is made of a nozzlematerial. Preferably, the nozzle material comprises a pre-compactifiedmaterial, for example with a density in a range of more than 95%, forexample from 98 to 100%, particularly preferably from 99 to 99.999%, ineach case based on the theoretical density of the nozzle material.Preferably, the nozzle material comprises a refractory metal, forexample molybdenum, tungsten or a combination thereof with a furtherrefractory metal. Molybdenum is a particularly preferred nozzlematerial. Preferably, a nozzle comprising molybdenum can have a densityof 100% of the theoretical density.

Preferably, the base plate comprised in a metal sheet crucible isthicker than the sides of the metal sheet crucible. Preferably, the baseplate is made of the same material as the sides of the metal sheetcrucible. Preferably, the base plate of the metal sheet crucible is nota rolled metal sheet. The base plate is for example 1.1 to 5000 times asthick or 2 to 1000 times as thick or 4 to 500 times as thick,particularly preferably 5 to 50 times as thick, each time compared witha wall of the metal sheet crucible.

According to a preferred embodiment of the first aspect of theinvention, the oven comprises a hanging or a standing sinter crucible.The silicon dioxide granulate is introduced into the hanging or standingsinter crucible and warmed to obtain a glass melt.

A sinter crucible means a crucible which is made from a sinter materialwhich comprises at least one sinter metal and has a density of not morethan 96% of the theoretical density of the metal. Sinter metal meansmetals of alloys which are obtained by sintering of metal powders. Thesinter material and the sinter metal in a sinter crucible are notrolled.

Preferably, the sinter material of the sinter crucible has a density of85% or more of the theoretical density of the sinter material, forexample a density from 85% to 95% or from 90% to 94%, particularlypreferably from 91% to 93%.

The sinter material can in principle be made of any material which isknown to the skilled person and which is suitable for melting silicondioxide. Preferably, the sinter material is made of at least one of theelements selected from the group consisting of refractory metals,graphite or materials lined with graphite foil.

Preferably, the sinter material comprises a first sinter metal selectedfrom the group consisting of molybdenum, tungsten and a combinationthereof. Furthermore, preferably, the sinter material additionallycomprises at least one further refractory metal which is different tothe first sinter metal particularly preferably selected from the groupconsisting of molybdenum, tungsten, rhenium, osmium, iridium, rutheniumor a combination of two or more thereof.

Preferably, the sinter material comprises an alloy of molybdenum with arefractory metal, or tungsten with a refractory metal. Particularlypreferable alloy metals are rhenium, osmium, iridium, ruthenium or acombination of two or more thereof. According to a further example, thesinter material comprises an alloy of molybdenum with tungsten, rhenium,osmium, iridium, ruthenium or a combination of two or more thereof. Forexample the sinter material can comprise an alloy of tungsten withmolybdenum, rhenium, osmium, iridium, ruthenium or a combination of twoor more thereof.

According to a further preferred embodiment, the above described sintermaterial can comprise a coating which comprises a refractory metal, inparticular rhenium, osmium, iridium, ruthenium or a combination of twoor more thereof. According to a preferred example, the coating comprisesrhenium, osmium, iridium, ruthenium, molybdenum or tungsten, or acombination of two or more thereof.

Preferably, the sinter material and its coating have differentcompositions. An example is a sinter material comprising molybdenumwhich is coated with one or more layers of rhenium, osmium, iridium,ruthenium, tungsten or of a combination of two or more thereof.According to another example, a sinter material comprising tungsten iscoated with one or more layers of rhenium, osmium, iridium, ruthenium,molybdenum or of a combination of two or more thereof. According toanother example, the sinter material can be made of molybdenum alloyedwith rhenium or of tungsten alloyed with rhenium, and coated on theinner side of the crucible with one or multiple layers comprisingrhenium, osmium, iridium, ruthenium or comprising a combination of twoor more thereof.

Preferably, a sinter crucible is made by sintering the sinter materialto obtain a mould. The sinter crucible can be made in a mould as awhole. It is also possible for individual parts of the sinter crucibleto be made in a mould and subsequently processed to obtain the sintercrucible. Preferably, the crucible is made out of more than one part,for example a base plate and one or more side parts. The side parts arepreferably made in one piece, based on the circumference of thecrucible. Preferably, the sinter crucible can be made of multiple sideparts arranged on top of each other. Preferably, the side parts of thesinter crucible are sealed by means of screwing or by means of a tongueand groove connection. A screwing is preferably achieved by making sideparts which have a thread at the borders. In the case of a tongue andgroove connection, two side parts which are to be joined each have anotch at the borders into which tongue is introduced as the connectingthird part, such that a form-closed connection is formed perpendicularto the plane of the crucible wall. Particularly preferably, a sintercrucible is made of more than one side part, for example of two or moreside parts, particularly preferably of three or more side parts. In thecase of the hanging sinter crucible, the parts are particularlypreferably screwed together. In the case of the standing sintercrucible, the parts are particularly preferably connected together bymeans of a tongue and groove connection.

The base plate can in principle be connected with the crucible wall byany means known to the skilled person and which is suitable for thispurpose. According to a preferred embodiment, the base plate has anoutward thread and the base plate is connected with the crucible wall bybeing screwed into it. According to a further preferred embodiment, thebase plate is connected with the crucible wall by means of screws.According to a further preferred embodiment, the base plate is suspendedin the sinter crucible, for example by laying the base plate on aninward flange of the crucible wall. According to a further preferredembodiment, at least a part of the crucible wall and a compactified baseplate are sintered in one piece. In the case of hanging sinter crucible,the base plate and crucible wall are particularly preferably screwedtogether. In the case the standing sinter crucible, the base plate andthe crucible wall are particularly preferably connected together bymeans of a tongue and groove connection.

Preferably, the base plate comprised by a sinter crucible is thickerthan the sides, for example 1.1 to 20 times as thick or 1.2 to 10 timesas thick or 1.5 to 7 times as thick, particularly preferably 2 to 5times as thick. Preferably, the sides have a constant wall thicknessover the circumference and over the height of the sinter crucible.

The sinter crucible has a nozzle. The nozzle is made of a nozzlematerial. Preferably, the nozzle material comprises a pre-compactifiedmaterial, for example with a density in a range of more than 95%, forexample from 98 to 100%, particularly preferably from 99 to 99.999%, ineach case based on the theoretical density of the nozzle material.Preferably, the nozzle material comprises a refractory metal, forexample molybdenum, tungsten or a combination therefrom with arefractory metal. Molybdenum is a particularly preferred nozzlematerial. Preferably, a nozzle comprising molybdenum can have a densityof 100% of the theoretical density.

The hanging sinter crucible can be heated in any way known to theskilled person and which appears to him to be suitable. The hangingsinter crucible can for example be heated inductively or resistively. Inthe case of inductive heating, the energy is introduced directly viacoils in the side wall of the sinter crucible and delivered from thereto the inside of the crucible. In the case of resistive heating, theenergy is introduced by radiation, whereby the solid surface is warmedfrom the outside and the energy is delivered from there to the inside.Preferably, the sinter crucible is heated inductively. For a resistiveheating, the energy is coupled via radiation, whereby the solid surfaceis warmed from outside and the energy is transferred from there to theinside. Preferably the melting crucible is heated inductively.

According to a preferred embodiment of the present invention, the energytransfer into the melting crucible, in particular for melting a bulkmaterial, is not performed by warming the melting crucible, or a bulkmaterial present therein, or both, using a flame, such as for example aburner flame directed into the melting crucible or onto the meltingcrucible.

Preferably, the sinter crucible has one or more than one heating zones,for example one or two or three or more than three heating zones,preferably one or two or three heating zones, particularly preferablyone heating zone. The heating zones of the sinter crucible can bebrought up to the same temperature or different temperatures. Forexample, all heating zones can be brought up to one temperature, or allheating zones can be brought up to different temperatures, or two ormore heating zones can be brought up to one temperature and one or moreheating zones can, independently of each other, be brought up to othertemperatures. Preferably, all heating zones are brought up to thedifferent temperatures, for example the temperature of the heating zonesincreases in the direction of the material transport of the silicondioxide granulate.

A hanging sinter crucible means a sinter crucible as previouslydescribed which is arranged hanging in an oven.

Preferably, the hanging sinter crucible has at least one, for example atleast two or at least three or at least four, particularly preferablyall of the following features:

-   -   {a} a hanging assembly, preferably a height adjustable hanging        assembly;    -   {b} at least two rings sealed together as side parts, preferably        at least two rings screwed to each other as side parts;    -   {c} a nozzle, preferably a nozzle which is permanently attached        to the crucible;    -   {d} a mandrel, for example a mandrel fixed to the nozzle with        pins or a mandrel fixed to the lid with a supporting rod or a        mandrel attached underneath the crucible with a supporting rod;    -   {e} at least one gas inlet, e.g. in the form of a filling pipe        or as a separate inlet, particularly preferably in the form of a        filling pipe;    -   {f} at least one gas outlet, e.g. at the lid or in the wall of        the crucible.    -   {g} A cooled jacket, particularly preferably a water cooled        jacket;    -   {h} An insulation on the outside of the crucible, for example on        the outside of the cooled jacket, preferably an insulation layer        made of zirconium oxide.

The hanging assembly is preferably a hanging assembly which is installedduring the construction of the hanging sinter crucible, for example ahanging assembly which is provided as an integral component of thecrucible, particularly preferably a hanging assembly which is providedout of the sinter material as an integral component of the crucible.Furthermore, the hanging assembly is preferably a hanging assembly whichis installed onto the sinter crucible and which is made of a materialwhich is different to the sinter material, for example of aluminium,steel, iron, nickel or copper, preferably of copper, particularlypreferably a cooled, for example a water cooled, hanging assembly madeof copper which is installed on the sinter crucible.

By virtue of the hanging assembly, the hanging sinter crucible can bemoved in the oven. Preferably, the crucible can be at least partiallyintroduced and withdrawn from the oven. If different heating zones arepresent in the oven, their temperature profile will be transferred tothe crucible which is present in the oven. By changing the position ofthe crucible in the oven, multiple heating zones, varying heating zonesor multiple varying heating zones can be produced in the crucible.

A standing sinter crucible means a sinter crucible of the typepreviously described which is arranged standing in an oven.

Preferably, the standing sinter crucible has at least one, for exampleat least two or at least three or at least four, particularly preferablyall of the following features:

-   -   /a/ A region formed as a standing area, preferably a region        formed as a standing area on the base of the crucible, further        preferably a region formed as a standing area in the base plate        of the crucible, particularly preferably a region formed as a        standing area at the outer edge of the base of the crucible;    -   /b/ at least two rings sealed together as side parts, preferably        at least two rings sealed together by means of a tongue and        groove connection as side parts;    -   /c/ a nozzle, preferably a nozzle which is permanently attached        to the crucible, particularly preferably a region of the base of        the crucible which is not formed as a standing area;    -   /d/ a mandrel, for example a mandrel fixed to the nozzle with        pins or a mandrel fixed to the lid with pins or a mandrel        attached from underneath the crucible with supporting rod;    -   /e/ at least one gas inlet, e.g. in the form of a filling tube        or as a separate inlet;    -   /f/ at least one gas outlet, e.g. as a separate outlet in the        lid or in the wall of the crucible;    -   /g/ a lid.

The standing sinter crucible preferably has a separation of the gascompartments in the oven and in the region underneath the oven. Theregion underneath the oven means the region underneath the nozzle, inwhich the removed glass melt is present. Preferably, the gascompartments are separated by the surface on which the crucible stands.Gas which is present in the gas compartment of the oven between theinner wall of the oven and the outer wall of the crucible, cannot leakdown into the region underneath the oven. The removed glass melt doesnot contact the gases from the gas compartment of the oven. Preferably,glass melts removed from an oven with a sinter crucible in a standingarrangement and quartz glass bodies formed therefrom have a highersurface purity than melts removed from an oven with a sinter crucible ina hanging arrangement and quartz glass bodies formed therefrom.

Preferably, the crucible is connected with the inlet and the outlet ofthe oven in such a way that silicon dioxide granulate can enter into thecrucible via the crucible inlet and through the inlet of the oven andglass melt can be removed through the outlet of the crucible and theoutlet of the oven.

Preferably, the crucible comprises, in addition to the at least oneinlet, at least one opening, preferably multiple openings, through whichthe gas can be introduced and removed. Preferably, the cruciblecomprises at least two openings, whereby at least one can be used as agas inlet and at least one can be used as a gas outlet. Preferably, theuse of at least one opening as gas inlet and at least one opening as gasoutlet leads to a gas flow in the crucible.

The silicon dioxide granulate is introduced into the crucible throughthe inlet of the crucible and subsequently warmed in the crucible. Thewarming can be carried out in the presence of a gas or of a gas mixtureof two or more gases. Furthermore, during the warming, water attached tothe silicon dioxide granulate can transfer to the gas phase and form afurther gas. The gas or the mixture of two or more gases is present inthe gas compartment of the crucible. The gas compartment of the cruciblemeans the region inside the crucible which is not occupied by a solid orliquid phase. Suitable gases are for example hydrogen, inert gases aswell as two or more thereof. Inert gases mean those gases which up to atemperature of 2400° C. do not react with the materials present in thecrucible. Preferred inert gases are nitrogen, helium, neon, argon,krypton and xenon, particularly preferably argon and helium. Preferably,the warming is carried out in reducing atmosphere. This can be providedby means of hydrogen or a combination of hydrogen and an inert gas, forexample a combination of hydrogen and helium, or of hydrogen andnitrogen, or of hydrogen and argon, particularly preferably acombination of hydrogen and helium.

Preferably, an at least partial gas exchange of air, oxygen and water inexchange for hydrogen, at least at least one inert gas, or in exchangefor a combination of hydrogen and at least one inert gas is carried outon the silicon dioxide granulate. The at least partial gas exchange iscarried out on the silicon dioxide granulate during introduction of thesilicon dioxide granulate, or before the warming, or during the warming,or during at least two of the aforementioned activities. Preferably, thesilicon dioxide granulate is warmed to melting in a gas flow of hydrogenand at least one inert gas, for example argon or helium.

Preferably, the dew point of the gas on exiting through the gas outletis less than 0° C.

The dew point means the temperature beneath which at fixed pressure apart of the gas or gas mixture in question condenses. In general, thismeans the condensation of water. The dew point is measured with a dewpoint mirror hygrometer according to the test method described in themethods section.

Preferably, the oven has at least one gas outlet, as does preferablyalso a melting crucible found therein, through which gas introduced intothe oven and gas formed during the running of the oven is removed. Theoven can additionally have at least one dedicated gas inlet.Alternatively or additionally, gas can be introduced through the inlet,also referred to as the solids inlet, for example together with thesilicon dioxide particles, or beforehand, afterwards, or by acombination of two or more of the aforementioned possibilities.

Preferably, the gas which is removed from the oven through the gasoutlet has a dew point of less than 0° C., for example of less than −10°C., or less than −20° C. on exiting from the oven through the gasoutlet. The dew point is measured according to the test method describedin the methods section at a slight overpressure of 5 to 20 mbar. Asuitable measuring device is for example an “Optidew” device from thecompany Michell Instruments GmbH, D-61381 Friedrichsdorf.

The dew point of the gas is preferably measured at a measuring locationat a distance of 10 cm or more from the gas outlet of the oven. Often,this distance is between 10 cm and 5 m. In this range of distances—herereferred to as “on exiting”—the distance of the measuring location fromthe gas outlet of the oven is insignificant for the result of the dewpoint measurement. The gas is conveyed to the measurement location byfluid connection, for example in a hose or a tube. The temperature ofthe gas at the measurement location is often between 10 and 60° C., forexample 20 to 50° C., in particular 20 to 30° C.

Suitable gases and gas mixtures have already been described. It wasestablished in the context of separate tests that the above disclosedvalues apply to each of the named gases and gas mixtures.

According to a further preferred embodiment, the gas or gas mixture hasa dew point of less than −50° C. prior to entering into the oven, inparticular into the melting crucible, for example less than −60° C., orless than −70° C., or less than −80° C. A dew point commonly does notexceed −60° C. Also, the following ranges for the dew point uponentering into the oven are preferred: from −50 to −100° C.; from −60 to−100° C. and from −70 to −100° C.

According to a further preferred embodiment, the dew point of the gasprior to entering into the oven is at least 50° C. less than on exitingfrom the melting crucible, for example at least 60° C., or even 80° C.For measuring the dew point on exiting from the melting crucible, theabove disclosures apply. For measuring the dew point prior to entry intothe oven, the disclosures apply analogously. Since no source ofcontribution to moisture is present and there is no possibility ofcondensing out between the measuring location and the oven, the distanceof the measuring location to the gas inlet of the oven is not relevant.

According to a preferred embodiment, the oven, in particular the meltingcrucible, is operated with a gas exchange rate in a range from 200 to3000 L/h.

According to a preferred embodiment, the dew point is measured in ameasuring cell, the measuring cell being separated by a membrane fromthe gas passing through the gas outlet. The membrane is preferablypermeable to moisture. By these means, the measuring cell can beprotected from dust and other particles present in the gas flow andwhich are conveyed out of the melting oven, in particular out of amelting crucible, along with the gas flow. By these means, the workingtime of a measuring probe can be increased considerably. The workingtime means the time period of operation of the oven during which neitherreplacement of the measuring probe, nor cleaning of the measuring probeis required.

According to a preferred embodiment, a dew point mirror measuring deviceis employed.

The dew point at the gas outlet of the oven can be configured.Preferably, a process for configuring the dew point at the outlet of theoven comprises the following steps:

-   -   I) Providing an input material in an oven, wherein the input        material has a residual moisture;    -   II) Operating the oven, wherein a gas flow is passed through the        oven, and    -   III) Varying the residual moisture of the input material, or the        gas replacement rate of the gas flow.

Preferably, this process can be used to configure the dew point to arange of less than 0° C., for example less than −10° C., particularlypreferably less than −20° C. Further preferably, the dew point can beconfigured to a range of less than 0° C. to −100° C., for example lessthan −10° C. to −80° C., particularly preferably less than −20° C. to−60° C.

For the preparation of a quartz glass body, “Input material” meanssilicon dioxide particles which are provided, preferably silicon dioxidegranulate, silicon dioxide grain, or combinations thereof. The silicondioxide particles, the granulate and the grain are preferablycharacterised by the features described in the context of the firstaspect.

The oven and the gas flow are preferably characterised by the featuresdescribed in the context of the first aspect. Preferably, the gas flowis formed by introducing a gas into the oven through an inlet and byremoving a gas out of the oven through an outlet. The “gas replacementrate” means the volume of gas which is passed out of the oven throughthe outlet per unit time. The gas replacement rate is also called thethroughput of the gas flow or volume throughput.

The configuration of the dew point can in particular be performed byvarying the residual moisture of the input material or the gasreplacement rate of the gas flow. For example, the dew point can beincreased by increasing residual moisture of the input material. Bydecreasing the residual moisture of the input material, the dew pointcan be reduced. An increase in the gas replacement rate can lead to areduction in the dew point. A reduced gas replacement rate on the otherhand can yield an increased dew point.

Preferably, the gas replacement rate of the gas flow is in a range from200 to 3000 L/h, for example 200 to 2000 L/h, particularly preferably200 to 1000 L/h.

The residual moisture of the input material is preferably in a rangefrom 0.001 wt. % to 5 wt. %, for example from 0.01 to 1 wt. %,particularly preferably 0.03 to 0.5 wt. %, in each case based on thetotal weight of the input material.

Preferably, the dew point can also be affected by further factors.Examples of such means are the dew point of the gas flow on entry intothe oven, the oven temperature and the composition of the gas flow. Areduction of the dew point of the gas flow on entry into the oven, areduction of the oven temperature or a reduction of the temperature ofthe gas flow at the outlet of the oven can lead to a reduction of thedew point of the gas flow at the outlet. The temperature of the gas flowat the outlet of the oven has no effect on the dew point, as long as itis above the dew point.

Particularly preferably, the dew point is configured by varying the gasreplacement rate of the gas flow.

Preferably, the process is characterised by at least one, for example atleast two or at least three, particularly preferably at least four ofthe following feature:

-   -   I} A residual moisture of the input material in a range from        0.001 to 5 wt. %, for example from 0.01 to 1 wt. %, particularly        preferably from 0.03 to 0.5 wt. %, in each case based on the        total weight of the input material.    -   II} A gas replacement rate of the gas flow in a range from 200        to 3000 L/h, for example from 200 to 2000 L/h, particularly        preferably from 200 to 1000 L/h;    -   III} An oven temperature in a range from 1700 to 2500° C., for        example in a range from 1900 to 2400° C., particularly        preferably in a range from 2100 to 2300° C.;    -   IV} A dew point of the gas flow on entry into the oven in a        range from −50° C. to −100° C., for example from −60° C. to        −100° C., particularly preferably from −70° C. to −100° C.;    -   V} The gas flow comprises helium, hydrogen or a combination        thereof, preferably helium and hydrogen in a ratio from 20:80 to        95:5;    -   VI} A temperature of the gas at the outlet in a range from 10 to        60° C., for example from 20 to 50° C., particularly preferably        from 20 to 30° C.

It is particularly preferred, when employing a silicon dioxide granulatewith a high residual moisture, to employ a gas flow with a high gasreplacement rate and a low dew point at the inlet of the oven. Bycontrast, when employing a silicon dioxide granulate with a low residualmoisture, a gas flow with a low gas replacement rate and a high dewpoint at the inlet of the oven can be used.

Particularly preferably, when employing a silicon dioxide granulate witha residual moisture of less than 3 wt. %, the gas replacement rate of agas flow comprising helium and hydrogen can be in a range from 200 to3000 L/h.

If a silicon dioxide granulate with a residual moisture of 0.1% is fedto the oven at 30 kg/h, a gas replacement rate of the gas flow in arange from 2800 to 3000 l/h is selected in the case of He/H₂=50:50 andin a range from 2700 to 2900 l/h is selected in the case of He/H₂=30:70,and a dew point of the gas flow before entry into the oven of −90° C. isselected. A dew point of less than 0° C. is thereby obtained at the gasoutlet.

If a silicon dioxide granulate with a residual moisture of 0.05% is fedto the oven at 30 kg/h, a gas replacement rate of the gas flow in arange from 1900 to 2100 l/h is selected in the case of He/H₂=50:50 andin a range from 1800 to 2000l/h is selected in the case of He/H₂=30:70,and a dew point of the gas flow before entry into the oven of −90° C. isselected. A dew point of less than 0° C. is thereby obtained at the gasoutlet.

If a silicon dioxide granulate with a residual moisture of 0.03% is fedto the oven at 30 kg/h, a gas replacement rate of the gas flow in arange from 1400 to 1600 l/h is selected in the case of He/H₂=50:50 andin a range from 1200 to 1400l/h is selected in the case of He/H₂=30:70,and a dew point of the gas flow before entry into the oven of −90° C. isselected. A dew point of less than 0° C. is thereby obtained at the gasoutlet.

According to the invention, the oven has at least a first and a furtherchamber joined to each other by a passage, the first and the furtherchamber having a different temperature, the temperature of the firstchamber being lower than the temperature of the further chamber. In thefurther chamber, a glass melt is formed from the silicon dioxidegranulate. This chamber is referred to as melting chamber in thefollowing. A chamber which is joined to the melting chamber via a ductbut which is upstream of it is also referred to as pre-heating section.An example is those in which at least one outlet is directly connectedwith the inlet of the melting chamber. The arrangement above may also bemade in independent ovens, in which case the melting chamber is amelting oven. In the further description, however, the term ‘meltingoven’ may be taken as being synonymous to the term ‘melting chamber’: sowhat is said concerning the melting oven may also be taken as applyingto the melting chamber and vice versa. The term ‘pre-heating section’means the same in both cases.

Preferably, the silicon dioxide granulate has a temperature in a rangefrom 20 to 1300° C. on entry into the oven.

According to a first embodiment, the silicon dioxide granulate is nottempered prior to entry into the melting chamber. The silicon dioxidegranulate has for example a temperature in a range from 20 to 40° C. onentry into the oven, particularly preferably from 20 to 30° C. Ifsilicon dioxide granulate II is provided according to step i.), itpreferably has a temperature on entry into the oven in a range from 20to 40° C., particularly preferably from 20 to 30° C.

According to another embodiment, the silicon dioxide granulate istempered up to a temperature in a range from 40 to 1300° C. prior toentry into the oven. Tempering means setting the temperature to aselected value. The tempering can in principle be carried out in any wayknown to the skilled person and known for the tempering of silicondioxide granulate. For example, the tempering can be carried out in anoven arranged separate from the melting chamber or in an oven connectedto the melting chamber.

Preferably, the tempering is carried out in a chamber connected to themelting chamber. Preferably, the oven therefore comprises a pre-heatingsection in which the silicon dioxide can be tempered. Preferably, thepre-heating section is itself a feed oven, particularly preferably arotary kiln. A feed oven means a heated chamber which, in operation,effects a movement of the silicon dioxide from an inlet of the feed ovento an outlet of the feed oven. Preferably, the outlet is directlyconnected to an inlet of the melting oven. In this way, the silicondioxide granulate can arrive from the pre-heating section into themelting oven without further intermediate steps or means.

It is further preferred that the pre-heating section comprises at leastone gas inlet and at least one gas outlet. Through the gas inlet, thegas can arrive in the interior, the gas chamber of the preheatingsection, and through the gas outlet it can be removed. It is alsopossible to introduce gas into the pre-heating section via the inlet ofthe pre-heating section for the silicon dioxide granulate. Also, gas canbe removed via the outlet of the pre-heating section and subsequentlyseparated from the silicon dioxide granulate. Furthermore, preferably,the gas can be introduced via the inlet for the silicon dioxidegranulate and a gas inlet of the pre-heating section, and removed viathe outlet of the pre-heating section and a gas outlet of thepre-heating section.

Preferably, a gas flow is produced in the pre-heating section by use ofthe gas inlet and of the gas outlet. Suitable gases are for examplehydrogen, inert gases as well as two or more thereof. Preferred inertgases are nitrogen, helium, neon, argon, krypton and xenon, particularlypreferably nitrogen and helium. Preferably, a reducing atmosphere ispresent in the pre-heating section. This can be provided in the form ofhydrogen or a combination of hydrogen and an inert gas, for example acombination of hydrogen and helium or of hydrogen and nitrogen,particularly preferably a combination of hydrogen and helium.Furthermore, preferably, an oxidising atmosphere is present in thepre-heating section. This can preferably be provided in the form ofoxygen or a combination of oxygen and one or more further gases, airbeing particularly preferable. Further preferably, it is possible of thesilicon dioxide to be tempered at reduced pressure in the preheatingsection.

For example, the silicon dioxide granulate can have a temperature onentry into the oven in a range from 100 to 1100° C. or from 300 to 1000or from 600 to 900° C. If silicon dioxide granulate II is providedaccording to step i.), it preferably has a temperature on entry into theoven in a range from 100 to 1100° C. or from 300 to 1000 or from 600 to900° C.

According to the invention, the oven comprises at least two chambers.Preferably, the oven comprises a first and at least one further chamber.The first and the further chamber are connected to each other by apassage.

The at least two chambers can in principle be arranged in the oven inany manner, preferably vertical or horizontal, particularly preferablyvertical. Preferably, the chambers are arranged in the oven in such away that on carrying out the process according to the first aspect ofthe invention, silicon dioxide granulate passes through the firstchamber and is subsequently heated in the further chamber to obtain aglass melt. The further chamber preferably has the above describedfeatures of the melting oven and of the crucible arranged therein.

Preferably, each of the chambers comprises an inlet and an outlet.Preferably, the inlet of the oven is connected to the inlet of the firstchamber via a passage. Preferably, the outlet of the oven is connectedto the outlet of the further chamber via a passage. Preferably, theoutlet of the first chamber is connected to the inlet of the furtherchamber via a passage.

Preferably, the chambers are arranged in such a manner that the silicondioxide granulate can arrive in the first chamber through the inlet ofthe oven. Preferably, the chambers are arranged in such a manner that asilicon dioxide glass melt can be removed from the further chamberthrough the outlet of the oven. Particularly preferably, the silicondioxide granulate can arrive in the first chamber through the inlet ofthe oven and a silicon dioxide glass melt can be removed from a furtherchamber through the outlet of the oven.

The silicon dioxide, in the form of granulate or powder, can go from afirst into a further chamber through the passage in the direction ofmaterial transport as defined by the process. Reference to chambersconnected by a passage includes arrangements in which furtherintermediate elements arrange in the direction of the material transportbetween a first and a further chamber. In principle, gases, liquids andsolids can pass through the passage. Preferably, silicon dioxide powder,slurries of silicon dioxide powder and silicon dioxide granulate canpass through the passage between a first and a further chamber. Whilstthe process according to the invention is carried out, all of thematerials introduced into the first chamber can arrive in the furtherchamber via the passage between the first and the further chamber.Preferably, only silicon dioxide in the form of granulate or powderarrive in the further chamber via the passage between the first and thefurther chamber. Preferably, the passage between the first and thefurther chamber is closed up by the silicon dioxide, such that the gaschamber of the first and the further chamber are separated from eachother, preferably such that in different gases or gas mixtures,different pressures or both can be present in the gas chambers.According to another preferred embodiment, the passage is formed of agate, preferably a rotary gate valve.

Preferably, the first chamber of the oven has at least one gas inlet andat least one gas outlet. The gas inlet can in principle have any formwhich is known to the skilled person and which is suitable forintroduction of a gas, for example a nozzle, a vent or a tube. The gasoutlet can in principle have any form known to the skilled person andwhich is suitable for removal of a gas, for example a nozzle, a vent ora tube.

Preferably, silicon dioxide granulate is introduced into the firstchamber through the inlet of the oven and warmed. The warming can becarried out in the presence of a gas or of a combination of two or moregases. To this end, the gas or the combination of two or more gases ispresent in the gas chamber of the first chamber. The gas chamber of thefirst chamber means the region of the first chamber which is notoccupied by a solid or liquid phase. Suitable gases are for examplehydrogen, oxygen, inert gases as well as two or more thereof. Preferredinert gases are nitrogen, helium, neon, argon, krypton and xenon,particularly preferred are nitrogen, helium and a combination thereof.Preferably, the warming is carried out in a reducing atmosphere. Thiscan preferably be provided in the form of hydrogen or a combination ofhydrogen and helium. Preferably, the silicon dioxide granulate is warmedin the first chamber in a flow of the gas or of the combination of twoor more gases.

It if further preferred that the silicon dioxide granulate is warmed inthe first chamber at reduced pressure, for example at a pressure of lessthan 500 mbar or less than 300 mbar, for example 200 mbar or less.

Preferably, the first chamber has at least one device with which thesilicon dioxide granulate is moved. In principle, all devices can beselected which are known to the skilled person for this purpose andwhich appear suitable. Preferably, stirring, shaking and slewingdevices.

According to a preferred embodiment, the first chamber of the oven is apre-heating section, particularly preferably a pre-heating section asdescribed above, which has the features as described above. Preferably,the pre-heating section is connected to the further chamber via apassage. Preferably, silicon dioxide goes from the pre-heating sectionvia a passage into the further chamber. The passage between thepre-heating section and the further chamber can be closed off, so thatno gases introduced into the pre-heating section go through the passageinto the further chamber. Preferably, the passage between thepre-heating section and the further chamber is closed off, so that thesilicon dioxide does not come into contact with water. The passagebetween the pre-heating section and the further chamber can be closedoff, so that the gas chamber of the pre-heating section and the firstchamber are separated from each other in such a way that different gasesor gas mixtures, different pressures or both can be present in the gaschambers. A suitable passage is preferably as per the above describedembodiments.

According to a further preferred embodiment, the first chamber of theoven is not a pre-heating section. For example, the first chamber can bea levelling chamber. A levelling chamber is a chamber of the oven inwhich variations in throughput in a pre-heating section upstreamthereof, or throughput differences between a pre-heating section and thefurther chamber are levelled. For example, as described above a rotarykiln can be arranged upstream of the first chamber. This commonly has athroughput which can vary by an amount up to 6% of the averagethroughput. Preferably, silicon dioxide is held in a levelling chamberat the temperature at which it arrives in the levelling chamber.

It is also possible for the oven to have a first chamber and more thanone further chambers, for example two further chambers or three furtherchambers or four further chambers or five further chambers or more thanfive further chambers, particularly preferably two further chambers. Ifthe oven has two further chambers, the first chamber is preferably apre-heating section, the first of the further chambers a levellingchamber and the second of the further chambers the melting chamber,based on the direction of the material transport.

According to a further preferred embodiment, an additive is present inthe first chamber. The additive is preferably selected from the groupconsisting of halogens, inert gases, bases, oxygen or a combination oftwo or more thereof.

In principle, halogens in elemental form and halogen compounds aresuitable additives. Preferred halogens are selected from the groupconsisting of chlorine, fluorine, chlorine containing compounds andfluorine containing compounds. Particularly preferable are elementalchlorine and hydrogen chloride.

In principle, all inert gases as well as mixtures of two or more thereofare suitable additives. Preferred inert gases are nitrogen, helium or acombination thereof.

In principle bases are also suitable additives. Preferred bases for useas additives are inorganic and organic bases.

Further, oxygen is a suitable additive. The oxygen is preferably presentas an oxygen containing atmosphere, for example in combination with aninert gas or a mixture of two or more inert gases, particularlypreferably in combination with nitrogen, helium or nitrogen and helium.

The first chamber can in principle comprise any material which is knownto the skilled person and which is suitable for heating silicon dioxide.Preferably, the first chamber comprises at least one element selectedfrom the group consisting of quartz glass, a refractory metal, aluminiumand a combination of two or more thereof, particularly preferably, thefirst chamber comprises quartz glass or aluminium.

Preferably, the temperature in the first chamber does not exceed 600° C.if the first chamber comprises a polymer or aluminium. Preferably, thetemperature in the first chamber is 100 to 1100° C., if the firstchamber comprises quartz glass. Preferably, the first chamber comprisesmainly quartz to glass.

In the transportation of the silicon dioxides from the first chamber tothe further chamber through the passage between the first and thefurther chamber, the silicon dioxide can in principle be present in anystate. Preferably, the silicon dioxide is present as a solid, forexample as particles, powder or granulate. According to a preferredembodiment of the first aspect of the invention, the transportation ofthe silicon dioxides from the first to the further chamber is carriedout as granulate.

The process as in one of the preceding claims, wherein the furtherchamber is a crucible made of a metal sheet or of a sinter material,wherein the sinter material comprises a sinter metal, wherein the metalsheet or the sinter metal is selected from the group consisting ofmolybdenum, tungsten and a combination thereof.

According to the invention, the temperatures in the first and furtherchambers are different. According to the invention, the temperature inthe first chamber is lower than the temperature in the further chamber.Preferably, the temperature difference between the first and furtherchambers is in a range from 600 to 2400° C., for example in a range from1000 to 2000° C. or from 1200 to 1800° C., particularly preferably in arange from 1500 to 1700° C. More preferably still, the temperature inthe first chamber is 600 to 2400° C., for example 1000 to 2000° C. or1200 to 1800° C., particularly preferably 1500 to 1700° C. lower thanthe temperature in the further chamber.

The temperature in the further chamber for melting the silicon dioxidegranulate lies preferably in the range from 1700 to 2500° C., forexample in the range from 1900 to 2400° C., particularly preferably inthe range from 2100 to 2300° C.

Preferably, the holding time in the further chamber is in a range fromone hour to 50 hours, for example one to 30 hours, particularlypreferably 5 to 20 hours. In the context of the present invention, theholding time means the time required to take a fill quantity from themelting chamber in accordance with the process while conducting theprocess as in the invention in the melting chamber in which the glassmelt is made. The fill quantity is the total mass of silicon dioxidepresent in the melting chamber, wherein the silicon dioxide may bepresent as a solid and as a glass melt.

Preferably, the temperature in the further chamber increases over thelength in the direction in which the material is transported.Preferably, the temperature in the further chamber increases over thelength in the direction in which the material is transported by at least100° C., for example by at least 300° C. or by at least 500° C. or by atleast 700° C., particularly preferably by at least 1000° C. Preferably,the maximum temperature in the oven is 1700 to 2500° C., for example1900 to 2400° C., particularly preferably 2100 to 2300° C. Thetemperature in the further chamber can increase uniformly or inaccordance with a temperature profile.

Preferably, the temperature in the further chamber reduces before theglass melt is removed from the oven. Preferably, the temperature in thefurther chamber reduces by 50 to 500° C., for example by 100° C. or by400° C., particularly preferably by 150 to 300° C. before the glass meltis removed from the oven. Preferably, the temperature of the glass meltwhen it is removed is 1750 to 2100° C., for example 1850 to 2050° C.,particularly preferably 1900 to 2000° C.

Preferably, the temperature in the further chamber falls over the lengthin the direction in which the material is transported and before theglass melt is removed from the oven. Preferably herein, the temperaturein the further chamber increases over the length in the direction inwhich the material is transported by at least 100° C., for example by atleast 300° C. or by at least 500° C. or by at least 700° C.,particularly preferably by at least 1000° C. Preferably, the maximumtemperature in the further chamber is 1700 to 2500° C., for example 1900to 2400° C., particularly preferably 2100 to 2300° C. Preferably, thetemperature in the further chamber before the glass melt is removed fromthe oven reduces by 50 to 500° C., for example by 100° C. or by 400° C.,particularly preferably by 150 to 300° C.

The glass melt is removed from the oven through the outlet, preferablyvia a nozzle.

Step iii.)

A quartz glass body is made out of at least a part of the glass melt.For this, preferably at least a part of the glass melt made in step ii)is removed and the quartz glass body is made out of it.

The removal of the part of the glass melt made in step ii) can inprinciple be carried out continuously from the melting oven or themelting chamber or after the production of the glass melt has beenfinished. Preferably, a part of the glass melt is removed continuously.The glass melt is removed through the outlet of the oven or through theoutlet of the melting chamber, preferably via a nozzle.

The glass melt can be cooled before, during or after the removal, to atemperature which enables the forming of the glass melt. A rise in theviscosity of the glass melt is connected to the cooling of the glassmelt. The glass melt is preferably cooled to such an extent that in theforming, the produced form holds and the forming is at the same time aseasy and reliable as possible and can be carried out with little effort.The skilled person can easily establish the viscosity of the glass meltfor forming by varying the temperature of the glass melt at the formingtool. Preferably, the glass melt has a temperature on removal in therange from 1750 to 2100° C., for example 1850 to 2050° C., particularlypreferably 1900 to 2000° C. Preferably, the glass melt is cooled to atemperature of less than 500° C. after removal, for example of less than200° C. or less than 100° C. or less than 50° C., particularlypreferably to a temperature in the range from 20 to 30° C.

The quartz glass body which is formed can be a solid body or a hollowbody. A solid body means a body which is mainly made out of a singlematerial. Nevertheless, a solid body can have one or more inclusions,e.g. gas bubbles. Such inclusions in a solid body commonly have a sizeof 65 mm³ or less, for example of less than 40 mm³, or of less than 20mm³, or of less than 5 mm³, or of less than 2 mm³, particularlypreferably of less than 0.5 mm³. Preferably, a solid body comprises lessthan 0.02 vol.-% of its volume as inclusion, for example less than 0.01vol.-% or less than 0.001 vol.-%, in each case based on the total volumeof the solid body.

The quartz glass body has an exterior form. The exterior form means theform of the outer edge of the cross section of the quartz glass body.The exterior form of the quartz glass body in cross-section ispreferably round, elliptical or polygonal with three or more corners,for example 4, 5, 6, 7 or 8 corners, particularly preferably the quartzglass body is round.

Preferably, the quartz glass body has a length in the range from 100 to10000 mm, for example from 1000 to 4000 mm, particularly preferably from1200 to 3000 mm.

Preferably, the quartz glass body has an exterior diameter in the rangefrom 1 to 500 mm, for example in a range from 2 to 400 mm, particularlypreferably in a range from 5 to 300 mm.

The forming of the quartz glass body is performed by means of a nozzle.The glass melt is sent through the nozzle. The exterior form of a quartzglass body formed through the nozzle is determined by the form of thenozzle opening. If the opening is round, a cylinder will be made informing the quartz glass body. If the opening of the nozzle has astructure, this structure will be transferred to the exterior form ofthe quartz glass body. A quartz glass body which is made by means of anozzle with structure at the opening, has an image of the structure inthe length direction along the glass strand.

The nozzle is integrated in the melting oven. Preferably, it isintegrated in the melting oven as part of the crucible, particularlypreferably as part of the outlet of the crucible.

Preferably, at least a part of the glass melt is removed through thenozzle. The exterior form of the quartz glass body is formed by theremoval of the at least part of the glass melt through the nozzle.

Preferably, the quartz glass body is cooled after the forming, so thatit maintains its form. Preferably, the quartz glass body is cooled afterthe forming to a temperature which is at least 1000° C. below thetemperature of the glass melt in the forming, for example at least 1500°C. or at least 1800° C., particularly preferably 1900 to 1950° C.Preferably, the quartz glass body is cooled to a temperature of lessthan 500° C., for example of less than 200° C. or less than 100° C. orless than 50° C., particularly preferably to a temperature in the rangefrom 20 to 30° C.

According to a preferred embodiment of the first aspect of theinvention, the obtained quartz glass body can be treated with at leastone procedure selected from the group consisting of chemical, thermal ormechanical treatment.

Preferably, the quartz glass body is chemically post treated. Posttreatment relates to treatment of a quartz glass body which has alreadybeen made. Chemical post treatment of the quartz glass body means inprinciple any procedure which is known to the skilled person and appearssuitable for employing materials for changing the chemical structure orthe composition of the surface of the quartz glass body, or both.Preferably, the chemical post treatment comprises at least one meansselected from the group consisting of treatment with fluorine compoundsand ultrasound cleaning.

Possible fluorine compounds are in particular hydrogen fluoride andfluorine containing acids, for example hydrofluoric acid. The liquidpreferably has a content of fluorine compounds in a range from 35 to 55wt.-%, preferably in a range from 35 to 45 wt.-%, the wt.-% in each casebased on the total amount of liquid. The remainder up to 100 wt.-% isusually water. Preferably, the water is fully desalinated water ordeionised water.

Ultrasound cleaning is preferably performed in a liquid bath,particularly preferably in the presence of detergents. In the case ofultrasound cleaning, commonly no fluorine compounds, for example neitherhydrofluoric acid nor hydrogen fluoride.

The ultrasound cleaning of the quartz glass body is preferably carriedout under at least one, for example at least two or at least three or atleast four or at least five, particularly preferably all of thefollowing conditions:

-   -   The ultrasound cleaning performed in a continuous process.    -   The equipment for the ultrasound cleaning has six chambers        connected to each other by tubes.    -   The holding time for the quartz glass body in each chamber can        be set. Preferably, the holding time of the quartz glass body in        each chamber is the same. Preferably, the holding time in each        chamber is in a range from 1 to 120 min, for example of less        than 5 min or from 1 to 5 min or from 2 to 4 min or of less than        60 min or from 10 to 60 min or from 20 to 50 min, particularly        preferably in a range from 5 to 60 min.    -   The first chamber comprises a basic medium, preferably        containing water and a base, and an ultrasound cleaner.    -   The third chamber comprises an acidic medium, preferably        containing water and an acid, and an ultrasound cleaner.    -   In the second chamber and in the fourth to sixth chamber, the        quartz glass body is cleaned with water, preferably with        desalinated water.    -   The fourth to sixth chambers are operated with cascades of        water. Preferably, the water is only introduced in the sixth        chamber and funs from the sixth chamber into the fifth and from        the fifth chamber into the fourth.

Preferably, the quartz glass body is thermally post treated. Thermalpost treatment of the quartz glass body means in principle a procedureknown to the skilled person and which appears suitable for changing theform or structure or both of the quartz glass body by means oftemperature.

Preferably, the thermal post treatment comprises at least a one meansselected from the group consisting of tempering, compressing, inflating,drawing, welding, and a combination of two or more thereof. Preferably,the thermal post treatment is not performed for the purpose of removingmaterial.

The tempering is preferably performed by heating the quartz glass bodyin an oven, preferably at a temperature in a range from 900 to 1300° C.,for example in a range from 900 to 1250° C. or from 1040 to 1300° C.,particularly preferably in a range from 1000 to 1050° C. or from 1200 to1300° C. Preferably, in the thermal treatment, a temperature of 1300° C.is not exceeded for continuous period of more than 1 h, particularlypreferably a temperature of 1300° C. is not exceeded during the entireduration of the thermal treatment. The tempering can in principle beperformed at reduced pressure, at normal pressure or at increasedpressure, preferably at reduced pressure, particularly preferably in avacuum.

The compressing is preferably performed by heating the quartz glassbody, preferably to a temperature of about 2100° C., and subsequentforming during a rotating turning motion, preferably with a rotationspeed of about 60 rpm. For example, a quartz glass body in the form of arod can be formed into a cylinder.

Preferably, a quartz glass body can be inflated by injecting a gas intothe quartz glass body. For example, a quartz glass body can by formedinto a large-diameter tube by inflating. For this, preferably the quartzglass body is heated to a temperature of about 2100° C., whilst arotating turning motion is performed, preferably with a rotation speedof about 60 rpm, and the interior is flushed with a gas, preferably at adefined and controlled inner pressure of up to about 100 mbar. Alarge-diameter tube means a tube with an outer diameter of at least 500mm.

A quartz glass body can preferably be drawn. The drawing is preferablyperformed by heating the quartz glass body, preferably to a temperatureof about 2100° C., and subsequently pulling with a controlled pullingspeed to the desired outer diameter of the quartz glass body. Forexample lamp tubes can be formed from quartz glass bodies by drawing.

Preferably, the quartz glass body is mechanically post treated. Amechanic post treatment of the quartz glass body means in principle anyprocedure known to the skilled person and which appears suitable forusing an abrasive means to change the shape of the quartz glass body orto split the quartz glass body into multiple pieces. In particular, themechanical post treatment comprises at least one means selected from thegroup consisting of grinding, drilling, honing, sawing, waterjetcutting, laser cutting, roughening by sandblasting, milling and acombination of two or more thereof.

Preferably, the quartz glass body is treated with a combination of theseprocedures, for example with a combination of a chemical and a thermalpost treatment or a chemical and a mechanical post treatment or athermal and a mechanical post treatment, particularly preferably with acombination of a chemical, a thermal and a mechanical post treatment.Furthermore, preferably, the quartz glass body can subjected to severalof the above mentioned procedures, each independently from the others.

According to an embodiment of the first aspect of the invention, theprocess comprises the following process step:

-   -   iv.) Making a hollow body with at least one opening from the        quartz glass body.

The hollow body which is made, has an interior and an exterior form.Interior form means the form of the inner edge of the cross section ofthe hollow body. The interior and exterior form in cross section of thehollow body can be the same or different. The interior and exterior formof the hollow body in cross section can be round, elliptical orpolygonal with three or more corners, for example 4, 5, 6, 7 or 8corners.

Preferably, the exterior form of the cross section corresponds to theinterior form of the hollow body. Particularly preferably, the hollowbody has in cross section a round interior and a round exterior form.

In another embodiment, the hollow body can differ in the interior andexterior form. Preferably, the hollow body has in cross section a roundexterior form and a polygonal interior form. Particularly preferably,the hollow body in cross section has a round exterior form and ahexagonal interior form.

Preferably, the hollow body has a length in the range from 100 to 10000mm, for example from 1000 to 4000 mm, particularly preferably from 1200to 2000 mm.

Preferably, the hollow body has a wall thickness in a range from 0.8 to50 mm, for example in a range from 1 to 40 mm or from 2 to 30 mm or from3 to 20 mm, particularly preferably in a range from 4 to 10 mm.

Preferably, the hollow body has an outer diameter of 2.6 to 400 mm, forexample in a range from 3.5 to 450 mm, particularly preferably in arange from 5 to 300 mm.

Preferably, the hollow body has an inner diameter of 1 to 300 mm, forexample in a range from 5 to 280 mm or from 10 to 200 mm, particularlypreferably in a range from 20 to 100 mm.

The hollow body comprises one or more openings. Preferably, the hollowbody comprises one opening. Preferably, the hollow body has an evennumber of openings, for example 2, 4, 6, 8, 10, 12, 14, 16, 18 or 20openings. Preferably, the hollow body comprises two openings.Preferably, the hollow body is a tube. This form of the hollow body isparticularly preferred if the light guide comprises only one core. Thehollow body can comprise more than two openings. The openings arepreferably located in pairs situated opposite each other at the ends ofthe quartz glass body. For example, each end of the quartz glass bodycan have 2, 3, 4, 5, 6, 7 or more than 7 openings, particularlypreferably 5, 6 or 7 openings. Preferred forms are for example tubes,twin tubes, i.e. tubes with two parallel channels, and multi-channeltubes, i.e. Tubes with more than two parallel channels.

The hollow body can in principle be formed by any method known to theskilled person. Preferably, the hollow body is formed by means of anozzle. Preferably, the nozzle comprises in the middle of its opening adevice which deviates the glass melt in the forming. In this way, ahollow body can be formed from a glass melt.

A hollow body can be made by the use a nozzle and subsequent posttreatment. Suitable post treatments are in principle all process knownto the skilled person for making a hollow body out of a solid body, forexample compressing channels, drilling, honing or grinding. Preferably,a suitable post treatment is to send the solid body over one or multiplemandrels, whereby a hollow body is formed. Also, the mandrel can beintroduced into the solid body to make a hollow body. Preferably, thehollow body is cooled after the forming.

Preferably, the hollow body is cooled to a temperature of less than 500°C. after the forming, for example less than 200° C. or less than 100° C.or less than 50° C., particularly preferably to a temperature in therange from 20 to 30° C.

Pre-Compacting

It is in principle possible to subject the silicon dioxide granulateprovided in step i.) to one or multiple pre-treatment steps, before itis warmed in step ii.) to obtain a glass melt. Possible pretreatmentsteps are for example thermal or mechanical treatment steps. For examplethe silicon dioxide granulate can be compactified before the warming instep ii.). “Compacting” means a reduction in the BET surface area and areduction of the pore volume.

The silicon dioxide granulate is preferably compactified by heating thesilicon dioxide granulate or mechanically by exerting a pressure to thesilicon dioxide granulate, for example rolling or pressing of thesilicon dioxide granulate. Preferably, the silicon dioxide granulate iscompactified by heating. Particularly preferably, the compacting of thesilicon dioxide granulate is performed by heating by means of apre-heating section which is connected to the melting oven.

Preferably, the silicon dioxide is compactified by heating at atemperature in a range from 800 to 1400° C., for example at atemperature in a range from 850 to 1300° C., particularly preferably ata temperature in a range from 900 to 1200° C.

In a preferred embodiment of the first aspect of the invention, the BETsurface area of the silicon dioxide granulate is not reduced to lessthan 5 m²/g prior to the warming in step ii.), preferably not to lessthan 7 m²/g or not to less than 10 m²/g, particularly preferably not toless than 15 m²/g. Furthermore, it is preferred, that the BET surfacearea of the silicon dioxide granulate is not reduced prior to thewarming in step ii.) compared with the silicon dioxide granulateprovided in step i.).

In a preferred embodiment of the first aspect of the invention, the BETsurface area of the silicon dioxide granulate is reduced to less than 20m²/g, for example to less than 15 m²/g, or to less than 10 m²/g, or to arange of more than 5 to less than 20 m²/g or from 7 to 15 m²/g,particularly preferably to a range of 9 to 12 m²/g. Preferably, the BETsurface area of the silicon dioxide granulate is reduced prior to theheating in step ii.) in comparison to the silicon dioxide granulateprovided in step i.) by less than 40 m²/g, for example by 1 to 20 m²/gor by 2 to 10 m²/g, particularly preferably by 3 to 8 m²/g, the BETsurface area after the compactification being more than 5 m²/g.

The compactified silicon dioxide granulate is referred to in thefollowing as silicon dioxide granulate III. Preferably, the silicondioxide granulate III has at least one, for example at least two or atleast three or at least four, particularly preferably at least five ofthe following features:

-   -   A. a BET surface area in a range of more than 5 to less than 40        m²/g, for example from 10 to 30 m²/g, particularly preferably in        a range of 15 to 25 m²/g;    -   B. a particle size D₁₀ in a range from 100 to 300 μm,        particularly preferably in a range from 120 to 200 μm;    -   C. a particle size D₅₀ in a range from 150 to 550 μm,        particularly preferably in a range from 200 to 350 μm;    -   D. a particle size D90 in a range from 300 to 650 μm,        particularly preferably in a range from 400 to 500 μm;    -   E. a bulk density in a range from 0.8 to 1.6 g/cm³, particularly        preferably from 1.0 to 1.4 g/cm³;    -   F. a tamped density in a range from 1.0 to 1.4 g/cm³,        particularly preferably from 1.15 to 1.35 g/cm³;    -   G. a carbon content of less than 5 ppm, for example of less than        4.5 ppm, particularly preferably of less than 4 ppm;    -   H. a Cl content of less than 500 ppm, particularly preferably        from 1 ppb to 200 ppm, wherein the ppm and ppb are each based on        the total weight of the silicon dioxide granulate III.

The silicon dioxide granulate III preferably has the feature combinationA./F./G. or A./F./H. or A./G./H., further preferably the featurecombination A./F./G./H.

The silicon dioxide granulate III preferably has the feature combinationA./F./G., wherein the BET surface area is in a range from 10 to 30 m²/g,The tamped density is in a range from 1.15 to 1.35 g/mL and the carboncontent is less than 4 ppm.

The silicon dioxide granulate III preferably has the feature combinationA./F./H., wherein the BET surface area is in a range from 10 to 30 m²/g,The tamped density is in a range from 1.15 to 1.35 g/mL and the chlorinecontent is in a range from 1 ppb to 200 ppm.

The silicon dioxide granulate III preferably has the feature combinationA./G./H., wherein the BET surface area is in a range from 10 to 30 m²/g,the carbon content is less than 4 ppm and the chlorine content is in arange from 1 ppb to 200 ppm.

The silicon dioxide granulate III preferably has the feature combinationA./F./G./H., wherein the BET surface area is in a range from 10 to 30m²/g, The tamped density is in a range from 1.15 to 1.35 g/mL, thecarbon content is less than 4 ppm and the chlorine content is in a rangefrom 1 ppb to 200 ppm.

Preferably, in at least one process step, a silicon component differentto silicon dioxide is introduced. The introduction of silicon componentsdifferent to silicon dioxide is also referred to in the following asSi-doping. In principle, the Si-doping can be performed in any processstep. Preferably, the Si-doping is preferred in step i.) or in stepii.).

The silicon component which is different to silicon dioxide can inprinciple be introduced in any form, for example as a solid, as aliquid, as a gas, in solution or as a dispersion. Preferably, thesilicon component different to silicon dioxide is introduced as apowder. Also, preferably, the silicon component different to silicondioxide can be introduced as a liquid or as a gas.

The silicon component which is different to silicon dioxide ispreferably introduced in an amount in a range from 1 to 100,000 ppm, forexample in a range from 10 to 10,000 ppm or from 30 to 1000 ppm or in arange from 50 to 500 ppm, particularly preferably in a range from 80 to200 ppm, further particularly preferably in a range from 200 to 300 ppm,in each case based on the total weight of silicon dioxide.

The silicon component which is different to silicon dioxide can besolid, liquid or gaseous. If it is solid, it preferably has a meanparticle size of up to 10 mm, for example of up to 1000 μm of up to 400μm or in a range from 1 to 400 μm, for example 2 to 200 μm or 3 to 100μm, particularly preferably in a range from 5 to 50 μm. The particlesize values are based on the state of the silicon component which isdifferent to silicon dioxide at room temperature.

The silicon component preferably has a purity of at least 99.5 wt.-%,for example at least 99.8 wt.-% or at least 99.9 wt.-%, or at least99.99 wt.-%, particularly preferably at least 99.999 wt. %, in each casebased on the total weight of the silicon component. Preferably, thesilicon component has a carbon content of not more than 10 ppm, forexample not more than 50 ppm, particularly preferably not more than 1ppm, in each case based on the total weight the silicon component.Particularly preferably, this applies to silicon employed as the siliconcomponent. Preferably, the silicon component has an amount of impuritiesselected from the group consisting of Al, Ca, Co, Cr, Cu, Fe, Ge, Hf, K,Li, Mg, Mn, Mo, Na, Nb, Ni, Ti, V, W, Zn, Zr of not more than 250 ppm,for example not more than 150 ppm, particularly preferably not more than100 ppm, in each case based on the total weight of the siliconcomponent. Particularly preferably, this applies where silicon isemployed as the silicon component.

Preferably, a silicon component which is different to silicon dioxide isintroduced in process step i.). Preferably, the silicon component whichis different to silicon dioxide is introduced during the processing ofthe silicon dioxide powder to obtain a silicon dioxide granulate (stepII.). For example the silicon component which is different to silicondioxide can be introduced before, during or after the granulation.

Preferably, the silicon dioxide can be Si-doped by introducing thesilicon component which is different to silicon dioxide to the slurrycomprising silicon dioxide powder. For example, the silicon componentwhich is different to silicon dioxide can be mixed with silicon dioxidepowder to and subsequently slurried, or the silicon component which isdifferent to silicon dioxide can be introduced into a slurry of silicondioxide powder a liquid and then slurried, or the silicon dioxide powdercan be introduced into a slurry or solution of the silicon componentwhich is different to silicon dioxide in a liquid and then slurried.

Preferably, the silicon dioxide can be Si-doped by introduction of thesilicon component which is different to silicon dioxide duringgranulation. It is in principle possible to introduce the siliconcomponent which is different to silicon dioxide at any point in timeduring the granulation. In the case of spray granulation, the siliconcomponent which is different to silicon dioxide can for example besprayed through the nozzle into the spray tower together with theslurry. In the case of roll granulation, the silicon component which isdifferent to silicon dioxide can preferably be introduced in solid formor as a slurry, for example after introducing the slurry into thestirring vessel.

Furthermore, preferably, the silicon dioxide can be Si-doped byintroduction of the silicon component which is different to silicondioxide after the granulation. For example, the silicon dioxide can bedoped during the treatment of the silicon dioxide granulate I to obtainsilicon dioxide granulate II, preferably by introducing the siliconcomponent which is different to silicon dioxide during the thermal ormechanical treatment of the silicon dioxide granulate I.

Preferably, the silicon dioxide granulate II is doped with the siliconcomponent which is different to silicon dioxide.

Furthermore, preferably, the silicon component which is different tosilicon dioxide can also be introduced during several of the abovementioned sections, in particular during and after the thermal ormechanical treatment of the silicon dioxide granulate I to obtain thesilicon dioxide granulate II.

The silicon component which is different to silicon dioxide can inprinciple be silicon or any silicon containing compound known to theskilled person and which has a reducing effect. Preferably, the siliconcomponent which is different to silicon dioxide is silicon, asilicon-hydrogen compound, for example a silane, a silicon-oxygencompound, for example silicon monoxide, or to a silicon-hydrogen-oxygencompound, for example disiloxane. Examples of preferred silanes aremonosilane, disilane, trisilane, tetrasilane, pentasilane, hexasilane,heptasilane higher homologous compounds as well as isomers of theaforementioned, and cyclic silanes like cyclopentasilane.

Preferably, a silicon component which is different to silicon dioxide isintroduced in process step ii.).

Preferably, the silicon component which is different to silicon dioxidecan be introduced directly into the melting crucible with the silicondioxide granulate. Preferably, silicon as the silicon component which isdifferent from silicon dioxide can be introduced into the meltingcrucible with the silicon dioxide granulate. The silicon is preferablyintroduced as powder, in particular with the particle size previouslygiven for the silicon component which is different to silicon dioxide.

Preferably, the silicon component which is different to silicon dioxideis added to the silicon dioxide granulate before introduction into themelting crucible. The addition can in principle be performed at any timeafter the formation of the granulate, for example in the pre-heatingsection, before or during the pre-compacting of the silicon dioxidegranulate II, or to the silicon dioxide granulate III.

A silicon dioxide granulate obtained by addition of a silicon componentwhich is different to silicon dioxide is referred to in the following as“Si-doped granulate”. Preferably, the Si-doped granulate has at leastone, for example at least two or at least three or at least four,particularly preferably at least five of the following features:

-   -   [1] a BET surface area in a range of more than 5 to less than 40        m²/g, for example from 10 to 30 m²/g, particularly preferably in        a range from 15 to 25 m²/g;    -   [2] a particle size D₁₀ in a range from 100 to 300 μm,        particularly preferably in a range from 120 to 200 μm;    -   [3] a particle size D₅₀ in a range from 150 to 550 μm,        particularly preferably in a range from 200 to 350 μm;    -   [4] a particle size D90 in a range from 300 to 650 μm,        particularly preferably in a range from 400 to 500 μm;    -   [5] a bulk density in a range from 0.8 to 1.6 g/cm³,        particularly preferably from 1.0 to 1.4 g/cm³;    -   [6] a tamped density in a range from 1.0 to 1.4 g/cm³,        particularly preferably from 1.15 to 1.35 g/cm³;    -   [7] a carbon content of less than 5 ppm, for example of less        than 4.5 ppm, particularly preferably of less than 4 ppm;    -   [8] a Cl content of less than 500 ppm, particularly preferably        from 1 ppb to 200 ppm;    -   [9] an Al content of less than 200 ppb, particularly preferably        from 1 ppb to 100 ppb;    -   [10] a metal content of metals which are different to aluminium,        of less than 1000 ppb, for example in a range from 1 to 400 ppb,        particularly preferably in a range from 1 to 200 ppb;    -   [11] a residual moisture content of less than 3 wt.-%, for        example in a range from 0.001 wt.-% to 2 wt.-%, particularly        preferably from 0.01 to 1 wt.-%;    -   wherein the wt.-%, ppm and ppb are each based on the total        weight of the Si-doped granulate.

In a preferred embodiment of the first aspect of the invention, themelting energy is transferred to the silicon dioxide granulate via asolid surface.

A solid surface means a surface which is different to the surface of thesilicon dioxide granulate and which does not melt or collapse at thetemperatures to which the silicon dioxide granulate is heated formelting. Suitable materials for the solid surface are for example thematerials which are suitable as crucible material.

The solid surface can in principle be any surface which is known to theskilled person and which is suitable for this purpose. For example thecrucible or a separate component which is not the crucible can be usedas the solid surface.

The solid surface can in principle be heated in any manner known to theskilled person and which is suitable for this purpose, in order totransfer the melting energy to the silicon dioxide granulate.Preferably, the solid surface is heated by resistive heating orinductive heating. In the case of inductive heating, the energy isdirectly coupled into the solid surface by means of coils and deliveredfrom there to its inner side. In the case of resistive heating, thesolid surface is warmed from the outer side and passes the energy fromthere to its inner side. In this connection, a heating chamber gas withlow heat capacity is advantageous, for example an argon atmosphere or anargon containing atmosphere. For example, the solid surface can beheated electrically or by firing the solid surface with a flame from theoutside. Preferably, the solid surface is heated to a temperature whichcan transfer an amount of energy to the silicon dioxide granulate and/orpart melted silicon dioxide granulate which is sufficient for meltingthe silicon dioxide granulate.

According to a preferred embodiment of the present invention, the energytransfer into the crucible is not performed by warming the crucible, ora bulk material present therein, or both, using a flame, such as forexample a burner flame directed into the crucible or onto the crucible.

If a separate component is used as the solid surface, this can bebrought into contact with the silicon dioxide granulate in any manner,for example by laying the component on the silicon dioxide granulate orby introducing the component between the granules of the silicon dioxidegranulate or by inserting the component between the crucible and thesilicon dioxide granulate or by a combination of two or more thereof.The component can be heated before, or during or before and during thetransfer of the melting energy..

Preferably, the melting energy is transferred to the silicon dioxidegranulate via the inner side of the crucible. In this case, the crucibleis heated enough so that the silicon dioxide granulate melts. Thecrucible is preferably heated resistively or inductively. The warmth istransferred from the outer side to the inner side of the crucible. Thesolid surface of the inner side of the crucible transfers the meltingenergy to the silicon dioxide granulate.

According to a further preferred embodiment of the present invention,the melting energy is not transferred to the silicon dioxide granulatevia a gas compartment. Furthermore, preferably, the melting energy isnot transferred to the silicon dioxide granulate by firing of thesilicon dioxide granulate with a flame. Examples of these excluded meansof transferring energy are directing one or multiple burner flames fromabove in the melting crucible, or onto the silicon dioxide, or both.

The above described process according to the first aspect of theinvention relates to the preparation of a quartz glass body.

Preferably, the quartz glass body has at least one of the followingfeatures, for example at least two or at least three or at least four,particularly preferably at least five of the following features:

-   -   A] an OH content of less than 500 ppm, for example of less than        400 ppm, particularly preferably of less than 300 ppm;    -   B] a chlorine content of less than 60 ppm, preferably of less        than 40 ppm, for example of less than 40 ppm or less than 2 ppm        or less than 0.5 ppm, particularly preferably of less than 0.1        ppm;    -   C] an aluminium content of less than 200 ppb, for example of        less than 100 ppb, particularly preferably of less than 80 ppb;    -   D] an ODC content of less than 5·10¹⁵/cm³, for example in a        range from 0.1·10¹⁵ to 3·10¹⁵/cm³, particularly preferably in a        range from 0.5·10¹⁵ to 2.0·10¹⁵/cm³;    -   E] a metal content of metals which are different to aluminium,        of less than 1 ppm, for example of less than 0.5 ppm,        particularly preferably of less than 0.1 ppm;    -   F] a viscosity (p=1013 hPa) in a range from log₁₀ (η(1250°        C.)/dPas)=11.4 to log₁₀ (q (1250° C.)/dPas)=12.9 and/or log₁₀        (η(1300° C.)/dPas)=11.1 to log₁₀ (η(1300° C.)/dPas)=12.2 and/or        log₁₀ (η(1350° C.)/dPas)=10.5 to log₁₀ (η(1350° C.)/dPas)=11.5;    -   G] a standard deviation of the OH content of not more than 10%,        preferably not more than 5%, based on the OH content A] of the        quartz glass body;    -   H] a standard deviation of the chlorine content of not more than        10%, preferably not more than 5%, based on the chlorine content        B] of the quartz glass body;    -   I] a standard deviation of the aluminium content of not more        than 10%, preferably not more than 5%, based on the aluminium        content C] of the quartz glass body;    -   J] a refractive index homogeneity of less than 10⁴;    -   K] a cylindrical form,    -   L] a tungsten content of less than 1000 ppb, for example of less        than 500 ppb or of less than 300 ppb or of less than 100 ppb or        in a range from 1 to 500 ppb or from 1 to 300 ppb, particularly        preferably in a range from 1 to 100 ppb;    -   M] a molybdenum content of less than 1000 ppb, for example of        less than 500 ppb or of less than 300 ppb or of less than 100        ppb or in a range from 1 to 500 ppb or from 1 to 300 ppb,        particularly preferably in a range from 1 to 100 ppb, wherein        the ppb and ppm are each based on the total weight of the quartz        glass body.

Preferably, the quartz glass body has a metal content of metalsdifferent to aluminium of less than 1000 ppb, for example of less than500 ppb, particularly preferably of less than 100 ppb, in each casebased on the total weight of the quartz glass body. Often however, thequartz glass body has a content of metals different to aluminium of atleast 1 ppb. Such metals are for example sodium, lithium, potassium,magnesium, calcium, strontium, germanium, copper, molybdenum, titanium,iron and chromium. This can for example be present as an element, as anion, or as part of a molecule or of an ion or of a complex.

The quartz glass body can comprise further constituents. Preferably, thequartz glass body comprises less than 500 ppm, for example less than 450ppm, particularly preferably less than 400 ppm of further constituents,the ppm in each case being base on the total weight of the quartz glassbody. Possible other constituents are for example carbon, fluorine,iodine, bromine and phosphorus. These can for example be present as anelement, as an ion or as part of a molecule, an ion or a complex. Oftenhowever, the quartz glass body has a content of further constituents ofat least 1 ppb.

Preferably, the quartz glass body comprises less than 5 ppm carbon, forexample less than 4.5 ppm, particularly preferably less than 4 ppm, ineach case based on the total weight of the quartz glass body. Oftenhowever, the quartz glass body has a carbon content of at least 1 ppb.

Preferably, the quartz glass body has a homogeneously distributed OHcontent, Cl content or Al content. An indicator of the homogeneity ofthe quartz glass body can be expressed as the standard deviation of OHcontent, Cl content or Al content. The standard deviation is the measureof the spread of the values of a variable from their arithmetic mean,here the OH content, chlorine content or aluminium content. Formeasuring the standard deviation, the content in the sample of thecomponent in question e.g. OH, chlorine or aluminium, is measured atleast seven measuring locations.

The quartz glass body preferably has the feature combination A]/B]/C] orA]/B]/D] or A]/B]/F], further preferred the feature combinationA]/B]/C]/D] or A]/B]/C]/F] or A]/B]/D]/F], further preferably thefeature combination A]/B]/C]/D]/F].

The quartz glass body preferably has the feature combination A]/B]/C],wherein The OH content is less than 400 ppm, the chlorine content isless than 100 ppm and the aluminium content is less than 80 ppb.

The quartz glass body preferably has the feature combination A]/B]/D],The OH content is less than 400 ppm, the chlorine content is less than100 ppm and the ODC content is in a range from 0.1·10¹⁵ to 3·10¹⁵/cm³.

The quartz glass body preferably has the feature combination A]/B]/F],wherein The OH content is less than 400 ppm, the chlorine content isless than 100 ppm and the viscosity (p=1013 hPa) is in a range fromlog₁₀ (η(1250° C.)/dPas)=11.4 to log₁₀ (η(1250° C.)/dPas)=12.9.

The quartz glass body preferably has the feature combinationA]/B]/C]/D], wherein The OH content is less than 400 ppm, the chlorinecontent is less than 100 ppm, the aluminium content is less than 80 ppband the ODC content is in a range from 0.110¹⁵ to 3·10¹⁵/cm³.

The quartz glass body preferably has the feature combinationA]/B]/C]/F], wherein The OH content is less than 400 ppm, the chlorinecontent is less than 100 ppm, the aluminium content is less than 80 ppband the viscosity (p=1013 hPa) is in a range from log₁₀ (η(1250°C.)/dPas)=11.4 to log₁₀ (η(1250° C.)/dPas)=12.9.

The quartz glass body preferably has the feature combinationA]/B]/D]/F], wherein The OH content is less than 400 ppm, the chlorinecontent is less than 100 ppm, the ODC content is in a range from0.1·10¹⁵ to 3·10¹⁵/cm³ and the viscosity (p=1013 hPa) is in a range fromlog₁₀ (q (1250° C.)/dPas)=11.4 to log₁₀ (η(1250° C.)/dPas)=12.9.

The quartz glass body preferably has the feature combinationA]/B]/C]/D]/F], wherein The OH content is less than 400 ppm, thechlorine content is less than 100 ppm, the aluminium content is lessthan 80 ppb and the ODC content is in a range from 0.1·10¹⁵ to3·10¹⁵/cm³ and the viscosity (p=1013 hPa) is in a range from log₁₀(η(1250° C.)/dPas)=11.4 to log₁₀ (η(1250° C.)/dPas)=12.9.

A second aspect of the present invention is a quartz glass bodyobtainable by the process according to the first aspect of theinvention.

Preferably, the quartz glass body has at least one of the followingfeatures, for example at least two or at least three or at least four,particularly preferably at least five of the following features:

-   -   A] an OH content of less than 500 ppm, for example of less than        400 ppm, particularly preferably of less than 300 ppm;    -   B] a chlorine content of less than 60 ppm, preferably of less        than 40 ppm, for example of less than 40 or less than 2 ppm or        less than 0.5 ppm, particularly preferably of less than 0.1 ppm;    -   C] an aluminium content of less than 200 ppb, for example of        less than 100 ppb, particularly preferably of less than 80 ppb;    -   D] an ODC content of less than 5·10¹⁵/cm³, for example in a        range from 0.1·10¹⁵ to 3·10¹⁵/cm³, particularly preferably in a        range from 0.5·10¹⁵ to 2.0·10¹⁵/cm³;    -   E] a metal content of metals which are different to aluminium,        of less than 1 ppm, for example of less than 0.5 ppm,        particularly preferably of less than 0.1 ppm;    -   F] a viscosity (p=1013 hPa) in a range from log₁₀ (η(1250°        C.)/dPas)=11.4 to log₁₀ (q (1250° C.)/dPas)=12.9 and/or log₁₀        (η(1300° C.)/dPas)=11.1 to log₁₀ (η(1300° C.)/dPas)=12.2 and/or        log₁₀ (η(1350° C.)/dPas)=10.5 to log₁₀ (η(1350° C.)/dPas)=11.5;    -   G] a standard deviation of the OH content of not more than 10%,        preferably not more than 5%, based on the OH content A] of the        quartz glass body;    -   H] a standard deviation of the chlorine content of not more than        10%, preferably not more than 5%, based on the chlorine content        B] of the quartz glass body;    -   I] a standard deviation of the aluminium content of not more        than 10%, preferably not more than 5%, based on the aluminium        content C] of the quartz glass body;    -   K] a cylindrical form;    -   L] a tungsten content of less than 1000 ppb, for example of less        than 500 ppb or of less than 300 ppb or of less than 100 ppb or        in a range from 1 to 500 ppb or from 1 to 300 ppb, particularly        preferably in a range from 1 to 100 ppb;    -   M] a molybdenum content of less than 1000 ppb, for example of        less than 500 ppb or of less than 300 ppb or of less than 100        ppb or in a range from 1 to 500 ppb or from 1 to 300 ppb,        particularly preferably in a range from 1 to 100 ppb,    -   wherein the ppb and ppm are each based on the total weight of        the quartz glass body.

A third aspect of the present invention is a process for the preparationof a light guide comprising the following steps:

-   -   A/ Providing        -   A1/ a hollow body with at least one opening obtainable by a            process according to the first aspect of the invention            comprising step iv.), or        -   A2/ a quartz glass body according to the second aspect of            the invention, wherein the quartz glass body is first            processed to obtain a hollow body with at least one opening;        -   B/ Introduction of one or multiple core rods into the quartz            glass body through the at least one opening to obtain a            precursor;        -   C/ Drawing the precursor from step B/in the warm to obtain a            light guide with one or multiple cores and a jacket M1.

Step A/

The quartz glass body provided in step A/ is a hollow body with at leastone opening. The quartz glass body provided in step A/ is preferablycharacterised by the features according to the second aspect of theinvention. The quartz glass body provided in step A/ is preferablyobtainable by a process according to the first aspect of the inventioncomprising as step iv.) the preparation of a hollow body out of thequartz glass body. Particularly preferably, the quartz glass body thusobtained has the features according to the second aspect of theinvention.

Step B/

One or multiple core rods are introduced through the at least oneopening of the quartz glass body (step B/). A core rod in the context ofthe present invention means an object which is designed to be introducedinto a jacket, for example a jacket M1, and processed to obtain a lightguide. The core rod has a core of quartz glass. Preferably, the core rodcomprises a core of quartz glass and jacket layer MO which surrounds thecore.

Each core rod has a form which is selected such that it fits into thequartz glass body. Preferably, the exterior form of the core rodcorresponds to the form of the opening of the quartz glass body.Particularly preferably, the quartz glass body is a tube and the corerod is a rod with a round cross section.

The diameter of the core rod is smaller than the inner diameter of thehollow body. Preferably, the diameter of the core rod is 0.1 to 3 mmsmaller than the inner diameter of the hollow body, for example 0.3 to2.5 mm smaller or 0.5 to 2 mm smaller or 0.7 to 1.5 mm smaller,particularly preferably 0.8 to 1.2 mm smaller.

Preferably, the ratio of the inner diameter of the quartz glass body tothe diameter of the core rod is in the range from 2:1 to 1.0001:1, forexample in the range from 1.8:1 to 1.01:1 or in the range from 1.6:1 to1.005:1 or in the range from 1.4:1 to 1.01:1, particularly preferably inthe range from 1.2:1 to 1.05:1.

Preferably, a region inside the quartz glass body which is not filled bythe core rod can be filled with at least one further component, forexample with a silicon dioxide powder or with a silicon dioxidegranulate.

It is also possible for a core rod which is already present in a furtherquartz glass body to be introduced into a quartz glass body. The furtherquartz glass body in this case has an outer diameter which is smallerthan the inner diameter of the quartz glass body. The core rod which isintroduced into the quartz glass body can also be presenting two or morefurther quartz glass bodies, for example in 3 or 4 or 5 or 6 or morefurther quartz glass bodies.

A quartz glass body with one or multiple core rods obtainable in thisway will be referred to in the following as “precursor”.

Step C/

The precursor is drawn in the warm (step C/). The obtained product is alight guide with one or multiple cores and at least one jacket M1.

Preferably, the drawing of the precursor is performed with a speed inthe range from 1 to 100 m/h, for example with a speed in the range from2 to 50 m/h or from 3 to 30 m/h. Particularly preferably, the drawing ofthe quartz glass body is performed with a speed in the range from 5 to25 m/h.

Preferably, the drawing is performed in the warm at a temperature of upto 2500° C., for example at a temperature in the range from 1700 to2400° C., particularly preferably at a temperature in the range from2100 to 2300° C.

Preferably, the precursor is sent through an oven which heats theprecursor from the outside.

Preferably, the precursor is stretched until the desired thickness ofthe light guide is achieved. Preferably, the precursor is stretched to1,000 to 6,000,000 times the length, for example to 10,000 to 500,000times the length or to 30,000 to 200,000 times the length, in each casebased on the length of the quartz glass body provided in step A/.Particularly preferably, the precursor is stretched to 100,000 to10,000,000 times the length, for example to 150,000 to 5,800,000 timesthe length or to 160,000 to 640,000 times the length or to 1,440,000 to5,760,000 times the length or to 1,440,000 to 2,560,000 times thelength, in each case based on the length of the quartz glass bodyprovided in step A/.

Preferably, the diameter of the precursor is reduced by the stretchingby a factor in a range from 100 to 3,500, for example in a range from300 to 3,000 or from 400 to 800 or from 1,200 to 2,400 or from 1,200 to1,600, in each case based on the diameter of the quartz glass bodyprovided in step A/.

The light guide, also referred to as light wave guide, can comprises anymaterial which is suitable for conducting or guiding electromagneticradiation, in particular light.

Conducting or guiding radiation means propagating the radiation over thelength extension of the light guide without significant obstruction orattenuation of the intensity of the radiation. For this, the radiationis coupled into the guide via one end of the light guide. Preferably,the light to guide conducts electromagnetic radiation at a wavelengthrange of 170 to 5000 nm. Preferably, the attenuation of the radiation bythe light guide in the wavelength range in question is in a range from0.1 to 10 dB/km. Preferably, the light guide has a transfer rate of upto 50 Tbit/s.

Der light guide preferably has a curl parameter of more than 6 m. Thecurl parameter in the context of the invention means the bending radiusof a fibre, e.g. of a light guide or of a jacket M1, which is present asa freely moving fibre free from external forces.

The light guide is preferably made to be pliable. Pliable in the contextof the invention means that the light guide is characterised by abending radius of 20 mm or less, for example of 10 mm or less,particularly preferably less than 5 mm or less. A bending radius meansthe smallest radius which can be formed without fracturing the lightguide and without impairing the ability of the light guide to conductradiation. An impairment is present where there is attenuation of morethan 0.1 dB of light sent through a bend in the light guide. Theattenuation is preferably applied at a reference wavelength of 1550 nm.

Preferably, the quartz is composed of silicon dioxide with less than 1wt.-% of other substances, for example with less than 0.5 wt.-% of othersubstances, particularly preferably with less than 0.3 wt.-% of othersubstances, in each case based on the total weight of the quartz.Furthermore, preferably, the quartz comprises at least 99 wt.-% silicondioxide, based on the total weight of the quartz.

The light guide preferably has an elongate form. The form of the lightguide is defined by its length extension L and its cross section Q. Thelight guide preferably has a round outer wall along its length extensionL. A cross section Q of the light guide is always determined in a planewhich is perpendicular to the outer wall of the light guide. If thelight guide is curved in the length extension L, then the cross sectionQ is determined perpendicular to the tangent at a point on the outerwall of the light guide. The light guide preferably has a diameter dL ina range from 0.04 to 1.5 mm. The light guide preferably has a length ina range from 1 m to 100 km.

According to the invention, the light guide comprises one or multiplecores, for example one core or two cores or three cores or four cores orfive cores or six cores or seven cores or more than seven cores,particularly preferably one core. Preferably, more than 90%, for examplemore than 95%, particularly preferably more than 98%, of theelectromagnetic radiation which is conducted through the light guide isconducted in the cores. For the transport of light in the cores, thepreferred wavelength ranges apply, as already given for the light guide.Preferably, the material of the core is selected from the groupconsisting of glass or quartz glass, or a combination of both,particularly preferably quartz glass. The cores can, independently ofeach other, be made of the same material or of different materials.Preferably, all of the cores are made of the same material, particularlypreferably of quartz glass.

Each core has a, preferably round, cross section Q_(K) and has anelongate form with length L_(K). The cross section Q_(K) of a core isindependent from the cross section Q_(K) of each other core. The crosssection Q_(K) of the cores can be the same or different. Preferably, thecross sections Q_(K) of all the cores are the same. A cross sectionQ_(K) of a core is always determined in a plane which is perpendicularto the outer wall of the core or the outer wall of the light guide. Ifthe core is curved in length extension, then the cross section Q_(K)will be perpendicular to the tangent at a point on the outer wall of thecore. The length L_(K) of a core is independent of the length L_(K) ofeach other core. The lengths L_(K) of the cores can be the same ordifferent. Preferably, the lengths L_(K) of all the cores are the same.Each core preferably has a length L_(K) in a range from 1 m to 100 km.Each core has a diameter d_(K). The diameter d_(K) of a core isindependent of the diameter d_(K) of each other core. The diametersd_(K) of the cores can be the same or different. Preferably, thediameters d_(K) of all the cores are the same. Preferably, the diameterd_(K) of each core is in a range from 0.1 to 1000 μm, for example from0.2 to 100 μm or from 0.5 to 50 μm, particularly preferably from 1 to 30μm.

Each core has at least one distribution of refractive indexperpendicular to the maximum extension of the core. “Distribution ofrefractive index” means the refractive index is constant or changes in adirection perpendicular to the maximum extension of the core. Thepreferred distribution of refractive index corresponds to a concentricdistribution of refractive index, for example to a concentric profile ofrefractive index in which a first region with the maximum refractiveindex is present in the centre of the core and which is surrounded by afurther region with a lower refractive index. Preferably, each core hasonly one refractive index distribution over its length L_(K). Thedistribution of refractive index of a core is independent of thedistribution of refractive index in each other core. The distributionsof refractive index of the cores can be the same or different.Preferably, the distributions of refractive index of all the cores arethe same. In principle, it is also possible for a core to have multipledifferent distributions of refractive index.

Each distribution of refractive index perpendicular to the maximumextension of the core has a maximum refractive index n_(K). Eachdistribution of refractive index perpendicular to the maximum extensionof the core can also have further lower refractive indices. The lowestrefractive index of the distribution of refractive index is preferablynot more than 0.5 smaller than the maximum refractive index n_(K) of thedistribution of refractive index. The lowest refractive index of thedistribution of refractive index is preferably 0.0001 to 0.15, forexample 0.0002 to 0.1, particularly preferably 0.0003 to 0.05, less thanthe maximum refractive index n_(K) of the distribution of refractiveindex.

Preferably, the core has a refractive index n_(K) in a range from 1.40to 1.60, for example in a range from 1.41 to 1.59, particularlypreferably in a range from 1.42 to 1.58, in each case measured at areference wavelength of λ_(r)=589 nm (sodium D-line), at a temperatureof 20° C. and at normal pressure (p=1013 hPa). For further details inthis regard, see the test methods section. The refractive index n_(K) ofa core is independent of the refractive index n_(K) of each other core.The refractive indices n_(K) of the cores can be the same or different.Preferably, the refractive indices n_(K) of all the cores are the same.

Preferably, each core of the light guide has a density in a range from1.9 to 2.5 g/cm³, for example in a range from 2.0 to 2.4 g/cm³,particularly preferably in a range from 2.1 to 2.3 g/cm³. Preferably,the cores have a residual moisture content of less than 100 ppb, forexample of less than 20 ppb or of less than 5 ppb, particularlypreferably of less than 1 ppb, in each case based on the total weight ofthe core. The density of a core is independent of the density of eachother core. The densities of the cores can be the same or different.Preferably, the densities of all cores are the same.

If a light guide comprises more than one core, then each core is,independently of the other cores, characterised by the above features.It is preferred for all cores to have the same features.

According to the invention, the cores are surrounded by at least onejacket M1. The jacket M1 preferably surrounds the cores over the entirelength of the cores. Preferably, the jacket M1 surrounds the cores forat least 95%, for example at least 98% or at least 99%, particularlypreferably 100% of the exterior surface, that is to say the entire outerwall, of the cores. Often, the cores are entirely surrounded by thejacket M1 up until the ends (in each case the last 1-5 cm). This servesto protect the cores from mechanical impairment.

The jacket M1 can comprise any material, including silicon dioxide,which has a lower refractive index than at least one point P along theprofile of the cross section Q_(K) of the core. Preferably, this atleast one point in the profile of the cross section Q_(K) of the core isthe point which lies at the centre of the core. Furthermore, preferably,the point P in the profile of the cross section of the core is the pointwhich has a maximum refractive index monax in the core. Preferably, thejacket M1 has a refractive index n_(M1) which is at least 0.0001 lowerthan the refractive index of the core n_(K) at the at least one point inthe profile of the cross section Q of the core. Preferably, the jacketM1 has a refractive index n_(M1) which is lower than the refractiveindex of the core n_(K) by an amount in the range from 0.0001 to 0.5,for example in a range from 0.0002 to 0.4, particularly preferably in arange from 0.0003 to 0.3.

The jacket M1 preferably has a refractive index n_(M1) in a range from0.9 to 1.599, for example in a range from 1.30 to 1.59, particularlypreferably in a range from 1.40 to 1.57. Preferably, the jacket M1 formsa region of the light guide with a constant refractive index n_(M1). Aregion with constant refractive index means a region in which therefractive index does not deviate from the mean of n_(M1) by more than0.0001.

In principle, the light guide can comprise further jackets. Particularlypreferably at least one of the further jackets, preferably several orall of them, a refractive index which is lower than the refractive indexn_(K) of each core. Preferably, the light guide has one or two or threeor four or more than four further jackets which surround the jacket M1.Preferably, further jackets which surround the jacket M1 have arefractive index which is lower than the refractive index n_(M1) of thejacket M1.

Preferably, the light guide has one or two or three or four or more thanfour further jackets which surround the cores and which are surroundedby the jacket M1, i.e. situated between the cores and the jacket M1.Furthermore, preferably, the further jackets situated between the coresand the jacket M1 have a refractive index which is higher than therefractive index n_(M1) of the jacket M1.

Preferably, the refractive index decreases from the core of the lightguide to the outermost jacket. The reduction in the refractive indexfrom the core to the outermost jacket can occur in steps orcontinuously. The reduction in the refractive index can have differentsections. Furthermore, preferably, the refractive index can be steppedin at least one section and be continuous in at least one other section.The steps can be of the same or different height. It is certainlypossible to arrange sections with increasing refractive index betweensections with decreasing refractive index.

The different refractive indices of the different jackets can forexample be configured by doping of the jacket M1, of the further jacketsand/or of the cores.

Depending on the manner of preparation of a core, a core can alreadyhave a first jacket layer M0 following it preparation. This jacket layerM0 which directly neighbours the core is sometimes also called anintegral jacket layer. The jacket layer M0 is situated closer to themiddle point of the core than the jacket M1 and, if they are present,the further jackets. The jacket layer M0 commonly does not serve forlight conduction or radiation conduction. Rather, the jacket layer M0serves more to keep the radiation inside the core where it istransported. The radiation which is conducted in the core is thuspreferably reflected at the interface from the core to the jacket layerM0. This interface from the core to the jacket layer M0 is preferablycharacterised by a change in refractive index. The refractive index ofthe jacket layer M0 is preferably lower than the refractive index n_(K)of the core. Preferably, the jacket layer M0 comprises the same materialas the core, but has a lower refractive index to the core on account ofdoping or of additives.

Preferably, at least the jacket M1 is made out of silicon dioxide andhas at least one, preferably several or all of the following features:

-   -   a) an OH content of less than 10 ppm, for example of less than 5        ppm, particularly preferably of less than 1 ppm;    -   b) a chlorine content of less than 60 ppm, preferably of less        than 40 ppm, for example of less than 20 or less than 2 ppm,        particularly preferably of less than 0.5 ppm;    -   c) an aluminium content of less than 200 ppb, preferably of less        than 100 ppb, for example of less than 80 ppb, particularly        preferably of less than 60 ppb;    -   d) an ODC content of less than 5·10¹⁵/cm³, for example in a        range from 0.1·10¹⁵ to 3·10¹⁵/cm³, particularly preferably in a        range from 0.5·10¹⁵ to 2.0·10¹⁵/cm³;    -   e) a metal content of metals which are different to aluminium,        of less than 1 ppm, for example of less than 0.5 ppm,        particularly preferably of less than 0.1 ppm;

f) a viscosity (p=1013 hPa) in a range from log₁₀ (η(1250°C.)/dPas)=11.4 to log₁₀ (q (1250° C.)/dPas)=12.9 and/or log₁₀ (η(1300°C.)/dPas)=11.1 to log₁₀ (η(1300° C.)/dPas)=12.2 and/or log₁₀ (η(1350°C.)/dPas)=10.5 to log₁₀ (η(1350° C.)/dPas)=11.5;

g) a curl parameter of more than 6 m;

h) a standard deviation of the OH content of not more than 10%,preferably not more than 5%, based on the OH content a) of the jacketM1;

i) a standard deviation of the chlorine content of not more than 10%,preferably not more than 5%, based on the chlorine content b) of thejacket M1;

j) a standard deviation of the aluminium content of not more than 10%,preferably not more than 5%, based on the aluminium content c) of thejacket M1;

k) a refractive index homogeneity of less than 1·10⁴;

-   -   l) a transformation point Tg in a range from 1150 to 1250° C.,        particularly preferably in a range from 1180 to 1220° C.,    -   wherein the ppb and ppm are each based on the total weight of        the jacket M1.

Preferably, the jacket has a refractive index homogeneity of less than1·10⁴. The refractive index homogeneity indicates the maximum deviationof the refractive index at each position of a sample, for example of ajacket M1 or of a quartz glass body, based on the mean value of all therefractive indices measured in the sample. For measuring the mean value,the refractive index is measured at least seven measuring locations.

Preferably, the jacket M1 has a metal content of metals different toaluminium of less than 1000 ppb, for example of less than 500 ppb,particularly preferably of less than 100 ppb, in each case based on thetotal weight of the jacket M1. Often however, the jacket M1 has acontent of metals different to aluminium of at least 1 ppb. Such metalsare for example sodium, lithium, potassium, magnesium, calcium,strontium, germanium, copper, molybdenum, titanium, iron and chromium.These can be present, for example, as an element, as an ion or as partof a molecule or of an ion or of a complex.

The jacket M1 can comprise further constituents. Preferably, the jacketcomprises less than 500 ppm, for example less than 450 ppm, particularlypreferably less than 400 ppm of further constituents, the ppm in eachcase based on the total weight of the jacket M1. Possible furtherconstituents are for example carbon, fluorine, iodine, bromine andphosphorus. These can be present for example as an element, as an ion oras part of a molecule, of an ion or of a complex. Often however, thejacket M1 has a content of further constituents of at least 1 ppb.

Preferably, the jacket M1 comprises less than 5 ppm carbon, for exampleless than 4 ppm or less than 3 ppm, particularly preferably less than 2ppm, in each case based on the total weight of the jacket M1. Oftenhowever, the jacket M1 has a carbon content of at least 1 ppb.

Preferably, the jacket M1 has a homogeneous distribution of OH content,Cl content or Al content.

In a preferred embodiment of the light guide, the jacket M1 contributesby weight at least 80 wt.-%, for example at least 85 wt.-%, particularlypreferably at least 90 wt.-%, in each case based on the total weight ofthe jacket M1 and the cores. Preferably, the jacket M1 contributes byweight at least 80 wt.-%, for example at least 85 wt.-%, particularlypreferably at least 90 wt. %, in each case based on the total weight ofthe jacket M1, the cores and the further jackets situated between thejacket M1 and the cores. Preferably, the jacket M1 contributes by weightat least 80 wt.-%, for example at least 85 wt.-%, particularlypreferably at least 90 wt.-%, in each case based on the total weight ofthe light guide.

Preferably, the jacket M1 has a density in a range from 2.1 to 2.3g/cm³, particularly preferably in a range from 2.18 to 2.22 g/cm³.

A further aspect relates to a light guide, obtainable by a processcomprising the following steps:

-   -   A/ Provision        -   A1/ of a hollow body with at least one opening obtainable by            a process according to the first aspect of the invention            comprising step iv.), or        -   A2/ of a quartz glass body according to the second aspect of            the invention, wherein the quartz glass body is first            processed to obtain a hollow body with at least one opening;    -   B/ Introduction of one or multiple core rods into the quartz        glass body through the at least one opening to obtain a        precursor;    -   C/ Drawing the precursor of step B/ in the warm to obtain a        light guide with one or multiple cores and a jacket M1.

The steps A/, B/ and C/ are preferably characterised by the featuresdescribed in the context of the third aspect of the invention.

The light guide is preferably characterised by the features described inthe context of the third aspect of the invention.

A fourth aspect of the present invention relates to a process for thepreparation of an illuminant comprising the following steps:

-   -   (i) Provision        -   (i-1) of a hollow body with at least one opening obtainable            by a process according to the first aspect of the invention            comprising step iv.); or        -   (i-2) of a quartz glass body according to the second aspect            of the invention, wherein the quartz glass body is first            processed to obtain a hollow body;    -   (ii) Optionally fitting the hollow body with electrodes;    -   (iii) Filling the hollow body with a gas.

Step (i)

In step (i), a hollow body is provided. The hollow body provided in step(i) comprises at least one opening, for example one opening or twoopening or three openings or four opening, particularly preferably oneopening or two openings.

Preferably, a hollow body with at least one opening is provided in step(i) which is obtainable by a process according to the first aspect ofthe invention comprising step iv.), (step (i-1)). Preferably, the hollowbody has the features described in the context of the first or secondaspect of the invention.

Preferably, a hollow body is provided in step (i) which is obtainablefrom a quartz glass body according to the second aspect of theinvention, (step (i-2)). There are many possibilities for processing aquartz glass body according to the second aspect of the invention toobtain a hollow body.

Preferably, a hollow body with two openings can be formed out of aquartz glass body analogue to step iv.) of the first aspect of theinvention.

The processing of the quartz glass body to obtain a hollow body with anopening can in principle be performed by means of any process known tothe skilled person and which are suitable for the preparation of glasshollow bodies with an opening. For example, processes comprising apressing, blowing, sucking or a combination thereof are suitable. It isalso possible to form a hollow body with one opening from a hollow bodywith two openings by closing an opening, for example by melting shut.

The obtained hollow body preferably has the features described in thecontext of the first and second aspects of the invention.

The hollow body is made of a material which comprises silicon dioxide,preferably in in a range from 98 to 100 wt.-%, for example in a rangefrom 99.9 to 100 wt.-%, particularly preferably 100 wt.-%, in each casebased on the total weight of the hollow body.

The material out of which the hollow body is prepared preferably has atleast one, preferably several, for example two, or preferably all of thefollowing features:

-   -   HK1. a silicon dioxide content of preferably more than 95 wt.-%,        for example more than 97 wt.-%, particularly preferably more        than 99 wt.-%, based on the total weight of the material;    -   HK2. a density in a range from 2.1 to 2.3 g/cm³, particularly        preferably in a range from 2.18 to 2.22 g/cm³;    -   HK3. a light transmissibility at at least one wavelength in the        visible range from 350 to 750 nm in a range from 10 to 100%, for        example in a range from 30 to 99.99%, particularly preferably in        a range from 50 to 99.9%, based on the amount of light which is        produced inside the hollow body;    -   HK4. an OH content of less than 500 ppm, for example of less        than 400 ppm, particularly preferably of less than 300 ppm;    -   HK5. a chlorine content of less than 60 ppm, preferably of less        than 40 ppm, for example of less than 40 ppm or less than 2 ppm        or less than 0.5 ppm, particularly preferably of less than 0.1        ppm;    -   HK6. an aluminium content of less than 200 ppb, for example of        less than 100 ppb, particularly preferably of less than 80 ppb;    -   HK7. a carbon content of less than 5 ppm, for example of less        than 4.5 ppm, particularly preferably of less than 4 ppm;    -   HK8. an ODC content of less than 5*10¹⁵/cm³;    -   HK9. a metal content of metals which are different to aluminium,        of less than 1 ppm, for example of less than 0.5 ppm,        particularly preferably of less than 0.1 ppm;    -   HK10. a viscosity (p=1013 hPa) in a range from log₁₀ q (1250°        C.)=11.4 to log₁₀ q (1250° C.)=12.9 and/or log₁₀ q (1300°        C.)=11.1 to log₁₀ q (1350° C.)=12.2 and/or log₁₀ q (1350°        C.)=10.5 to log₁₀ q (1350° C.)=11.5; HK11. A transformation        point Tg in a range from 1150 to 1250° C., particularly        preferably in a range from 1180 to 1220° C.;    -   wherein the ppm and ppb are each based on the total weight of        the hollow body.

Step (ii)

Preferably, the hollow body of step (i) is fitted with electrodes,preferably with two electrodes, before filling with a gas. Preferably,the electrodes are connected to a source of electrical current.Preferably, the electrodes are connected to an illuminant socket.

The material of the electrodes is preferably selected from the group ofmetals. In principle the electrode material can be selected from anymetal which does not oxidise, corrode, melt or otherwise become impairedin its form or conductivity as electrode under the operative conditionsof the illuminant. The electrode material is preferably selected fromthe group consisting of iron, molybdenum, copper, tungsten, rhenium,gold and platinum or at least two selected therefrom, tungsten,molybdenum or rhenium being preferred.

Step (iii)

The hollow body provided in step (i) and optionally fitted withelectrodes in step (ii) is filled with a gas.

The filling can be performed in any process known to the skilled personand which is suitable for the filling. Preferably, a gas is fed into thehollow body through the at least one opening.

Preferably, the hollow body is evacuated prior to filling with the gas,preferably evacuated to a pressure of less than 2 mbar. By subsequentintroduction of a gas, the hollow body is filled with the gas. Thesesteps can be repeated in order to reduce air impurities, in particularoxygen. Preferably, these steps are repeated at least twice, for exampleat least thrice or at least four times, particularly preferably at leastfive times until the amount of other gas impurities such as air, inparticular oxygen, is sufficiently low. This procedure is particularlypreferred for filling hollow bodies with one opening.

In the hollow body comprises two or more openings, the hollow body ispreferably filled through one of the openings. The air present in thehollow body prior to filling with the gas can exit through the at leastone further opening. The gas is fed through the hollow body until theamount of other gas impurities such as air, in particular oxygen, issufficiently low.

Preferably, the hollow body is filled with an inert gas or with acombination of two or more inert gases, for example with nitrogen,helium, neon, argon, krypton, xenon or a combination of two or morethereof, particularly preferably with krypton, xenon or a combination ofnitrogen and argon. Further preferred filling materials for the hollowbody of illuminants are deuterium and mercury.

Preferably, the hollow body is closed after filling a gas, so that thegas does not exit during the further processing, so that no air entersfrom outside during the further processing, or both. The closing can beperformed by melting or placing a cap. Suitable caps are for examplequartz glass caps, which are for example melted onto the hollow body, orilluminant sockets. Preferably, the hollow body is closed by melting.

The illuminant according to the fourth aspect of the invention comprisesa hollow body and optionally electrodes. The illuminant preferably hasat least one, for example at least two or at least three or at leastfour, particularly preferably at least five of the following features:

-   -   i. a volume in a range from 0.1 cm³ to 10 m³, for example in a        range from 0.3 cm³ to 8 m³, particularly preferably in a range        from 0.5 cm³ to 5 m³;    -   ii. a length in a range from 1 mm to 100 m, for example in a        range from 3 mm to 80 m, particularly preferably in a range from        5 mm to 50 m;    -   iii. an angle of radiation in a range from 2 to 360°, for        example in a range from 10 to 360°, particularly preferably in a        range from 30 to 360′;    -   iv. a radiation of light in a wavelength range from 145 to 4000        nm, for example in a range from 150 to 450 nm, or from 800 to        4000 nm, particularly preferably in a range from 160 to 280 nm;    -   v. a powder in a range from 1 mW to 100 kW, particularly        preferably in a range from 1 kW to 100 kW, or in a range from 1        to 100 Watt.

A further aspect relates to an illuminant, obtainable by a processcomprising the following steps:

-   -   (i) Providing:        -   (i-1) a hollow body with at least one opening obtainable by            a process according to the first aspect of the invention            comprising step iv.); or        -   (i-2) a quartz glass body according to the second aspect of            the invention, wherein the quartz glass body is first            processed to obtain a hollow body;    -   (ii) Optionally fitting the hollow body with electrodes;    -   (iii) Filling the hollow body with a gas.

The steps (i), (ii) and (iii) are preferably characterised by thefeatures described in the context of the fourth aspect.

The illuminant is preferably characterised by the features described inthe context of the fourth aspect.

A fifth aspect of the present invention relates to a process for thepreparation of a formed body comprising the following steps:

-   -   (1) Providing a quartz glass body according to the first or        second aspect of the invention;    -   (2) Forming the quartz glass body to obtain the formed body.

The quartz glass body provided in step (1) is a quartz glass bodyaccording to the second aspect of the invention or obtainable by aprocess according to the first aspect of the invention. Preferably, theprovided quartz glass body has the features of the first or secondaspect of the invention.

Step (2)

For forming the quartz glass body provided in step (1), in principle anyprocesses known to the skilled person and which are suitable for formingquartz glass are possible. Preferably, the quartz glass body is formedas described in the context of the first, third and fourth aspects ofthe invention to obtain a formed body. Furthermore, preferably, theformed body can be formed by means of techniques known to glass blowers.

The formed body can in principle take any shape which is formable out ofquartz glass. Preferred formed bodies are for example:

-   -   hollow bodies with at least one opening such as round bottomed        flasks and standing flasks,    -   fixtures and caps for such hollow bodies,    -   open articles such as bowls and boats (wafer carrier),    -   crucibles, arranged either open or closable,    -   sheets and windows,    -   cuvettes,    -   tubes and hollow cylinders, for example reaction tubes, section        tubes, cuboid chambers,    -   rods, bars and blocks, for example in round or angular,        symmetric or asymmetric format,    -   tubes and hollow cylinders closed off at one end or both ends,    -   domes and bells,    -   flanges,    -   lenses and prisms,    -   parts welded to each other,    -   curved parts, for example convex or concave surfaces and sheets,        curved rods and tubes.

According to a preferred embodiment, the formed body can be treatedafter the forming. For this, in principle all processes described inconnection with the first aspect of the invention which are suitable forpost treatment of the quartz glass body are possible. Preferably, theformed body can be mechanically processed, for example by drilling,honing, external grinding, reducing in size or drawing.

A further aspect relates to a formed body obtainable by a processcomprising the following steps:

-   -   (1) Providing a quartz glass body according to the first or        second aspect of the invention;    -   (2) Forming the quartz glass body to obtain the formed body.

The steps (1) and (2) are preferably characterised by the featuresdescribed in the context of the fifth aspect.

The formed body is preferably characterised by the features described inthe context of the fifth aspect.

FIGURES

FIG. 1 flow diagram (process for the preparation of a quartz glass body)

FIG. 2 flow diagram (process for the preparation of a silicon dioxidegranulate I)

FIG. 3 flow diagram (process for the preparation of a silicon dioxidegranulate II)

FIG. 4 flow diagram (process for the preparation of a light guide)

FIG. 5 flow diagram (process for the preparation of an illuminant)

FIG. 6 schematic representation of a hanging crucible in an oven

FIG. 7 schematic representation of a standing crucible in an oven

FIG. 8 schematic representation of a crucible with a flushing ring

FIG. 9 schematic representation of a spray tower

FIG. 10 schematic representation of a cross section of a light guide

FIG. 11 schematic representation of a view of a light guide

FIG. 12 schematic representation of a crucible with a dew pointmeasuring device

FIG. 13 schematic representation of a gas pressure sinter oven (GDSoven)

FIG. 14 flow diagram (process for the preparation of a formed body)

DESCRIPTION OF THE FIGURES

FIG. 1 shows a flow diagram containing the steps 101 to 104 of a process100 for the preparation of a quartz glass body according to the presentinvention. In a first step 101, a silicon dioxide granulate is provided.In a second step 102, a glass melt is made from the silicon dioxidegranulate.

Preferably, moulds are used for the melting which can be introduced intoand removed from an oven. Such moulds are often made of graphite. Theyprovide a negative form for the caste item. The silicon dioxidegranulate is filled into the mould and is first melted in the mould instep 103. Subsequently, the quartz glass body is formed in the samemould by cooling the melt. It is then freed from the mould and processedfurther, for example in an optional step 104. This procedure isdiscontinuous. The forming of the melt is preferably performed atreduced pressure, in particular in a vacuum. Further, it is possibleduring step 103 to charge the oven intermittently with a reducing,hydrogen containing atmosphere.

In another procedure, hanging or standing crucibles are preferablyemployed. The melting is preferably performed in a reducing, hydrogencontaining atmosphere. In a third step 103, a quartz glass body isformed. The formation of the quartz glass body is preferably performedby removing at least a part of the glass melt from the crucible andcooling. The removal is preferably performed through a nozzle at thelower end of the crucible. In this case, the form of the quartz glassbody can be determined by the design of the nozzle. In this way, forexample, solid bodies can be obtained. Hollow bodies are obtained forexample if the nozzle additionally has a mandrel. This example of aprocess for the preparation of quartz glass bodies, and in particularstep 103, is preferably performed continuously. In an optional step 104,a hollow body can be formed from a solid quartz glass body.

FIG. 2 shows a flow diagram containing the steps 201, 202 and 203 of aprocess 200 for the preparation of a silicon dioxide granulate I. In afirst step 201, a silicon dioxide powder is provided. A silicon dioxidepowder is preferably obtained from a synthetic process in which asilicon containing material, for example a siloxane, a silicon alkoxideor a silicon halide is converted into silicon dioxide in a pyrogenicprocess. In a second step 202, the silicon dioxide powder is mixed witha liquid, preferably with water, to obtain a slurry. In a third step203, the silicon dioxide contained in the slurry is transformed into asilicon dioxide granulate. The granulation is performed by spraygranulation. For this, the slurry is sprayed through a nozzle into aspray tower and dried to obtain granules, wherein the contact surfacebetween the nozzle and the slurry comprises a glass or a plastic.

FIG. 3 shows a flow diagram containing the steps 301, 302, 303 and 304of a process 300 for the preparation of a silicon dioxide granulate II.The steps 301, 302 and 303 proceed corresponding to the steps 201, 202and 203 according to FIG. 2. In step 304, the silicon dioxide granulateI obtained in step 303 is processed to obtain a silicon dioxidegranulate II. This is preferably performed by warming the silicondioxide granulate I in a chlorine containing atmosphere.

FIG. 4 shows a flow diagram containing the steps 401, 403 and 404 aswell as the optional step 402 of the process for the preparation of alight guide. In the first step 401, a quartz glass body is provided,preferably a quartz glass body prepared according to process 100. Such aquartz glass body can be a solid or a hollow quartz glass body. In asecond step 402, a hollow quartz glass body corresponding to step 104 isformed from a solid quartz glass body provided in step 401. In a thirdstep 403, one or more than one core rods are introduced into the hollow.In a fourth step 404, the quartz glass body fitted with one or more thanone core rods is processed to obtain a light guide. For this, the quartzglass body fitted with one or more than one core rods is preferablysoftened by warming and stretched until the desired thickness of thelight guide is achieved.

FIG. 5 shows a flow diagram containing the steps 501, 503 and 504 aswell as the optional step 502 of a process for the preparation of anilluminant. In the first step 501, a quartz glass body is provided,preferably a quartz glass body prepared according to process 100. Such aquartz glass body can be a solid or a hollow quartz glass body. If thequartz glass body provided in step 501 is solid, it is optionally formedin a second step 502 to obtain a hollow quartz glass body correspondingto step 104. In an optional third step, the hollow quartz glass body isfitted with electrodes. In a fourth step 504, the hollow quartz glassbody is filled with a gas, preferably with argon, krypton, xenon or acombination thereof. Preferably, a solid quartz glass body is firstprovided (501), formed to obtain a hollow body (502), fitted withelectrodes (503) and filled with a gas (504).

In FIG. 6, a preferred embodiment of an oven 800 with a hanging crucibleis shown. The crucible 801 is arranged hanging in the oven 800. Thecrucible 801 has a hanger assembly 802 in its upper region, as well as asolids inlet 803 and a nozzle 804 as outlet. The crucible 801 is filledvia the solids inlet 803 with silicon dioxide granulate 805. Inoperation, silicon dioxide granulate 805 is present in the upper regionof the crucible 801, whilst a glass melt 806 is present in the lowerregion of the crucible. The crucible 801 can be heated by heatingelements 807 which are arranged on the outer side of the crucible wall810. The oven also has an insulation layer 809 between the heatingelements 807 and the outer wall 808 of the oven. The space in betweenthe insulation layer 809 and the crucible wall 810 can be filled with agas and for this purpose has a gas inlet 811 and a gas outlet 812. Aquartz glass body 813 can be removed from the oven through the nozzle804.

In FIG. 7 a preferred embodiment of an oven 900 with a standing crucibleis shown. The crucible 901 is arranged standing in the oven 900. Thecrucible 901 has a standing area 902, a solids inlet 903 and a nozzle904 as outlet. The crucible 901 is filled with silicon dioxide granulate905 via the inlet 903. In operation, silicon dioxide granulate 905 ispresent in the upper region of the crucible, whilst a glass melt 906 ispresent in the lower region of the crucible. The crucible can be heatedby heating elements 907 which are arranged on the outer side of thecrucible wall 910. The oven also has an insulation layer 909 between theheating elements 907 and the outer wall 908. The space between theinsulation layer 909 and the crucible wall 910 can be filled with a gasand for this purpose has a gas inlet 911 and a gas outlet 912. A quartzglass body 913 can be removed from the crucible 901 through the nozzle904.

In FIG. 8 is shown a preferred embodiment of a crucible 1000. Thecrucible 1000 has a solids inlet 1001 and a nozzle 1002 as outlet. Thecrucible 1000 is filled with silicon dioxide granulate 1003 via thesolids inlet 1001. In operation, silicon dioxide granulate 1003 ispresent as a reposing cone 1004 in the upper region of the crucible1000, whilst a glass melt 1005 is present in the lower region of thecrucible. The crucible 1000 can be filled with a gas. It has a gas inlet1006 and a gas outlet 1007. The gas inlet is a flushing ring mounted onthe crucible wall above the silicon dioxide granulate. The gas in theinterior of the crucible is released through the flushing ring (with agas feed not shown here) close above the melting level and/or thereposing cone near the crucible wall and flows in the direction of thegas outlet 1007 which is arranged as a ring in the lid 1008 of thecrucible 1000. The gas flow 1010 which is produced in this way movesalong the crucible wall and submerges it. A quartz glass body 1009 canbe removed from the crucible 1000 through the nozzle 1002.

In FIG. 9 is shown a preferred embodiment of a spray tower 1100 forspray granulating silicon dioxide. The spray tower 1100 comprises a feed1101 through which a pressurised slurry containing silicon dioxidepowder and a liquid are fed into the spray tower. At the end of thepipeline is a nozzle 1102 through which the slurry is introduced intothe spray tower as a finely spread distribution. Preferably, the nozzleslopes upward, so that the slurry is sprayed into the spray tower asfine droplets in the nozzle direction and then falls down in an arcunder the influence of gravity. At the upper end of the spray towerthere is a gas inlet 1103. By introduction of a gas through the gasinlet 1103, a gas flow is created in the opposite direction to the exitdirection of the slurry out of the nozzle 1102. The spray tower 1100also comprises a screening device 1104 and a sieving device 1105.Particles which are smaller than a defined particle size are extractedby the screening device 1104 and removed through the discharge 1106. Theextraction strength of the screening device 1104 can be configured tocorrespond to the particle size of the particles to be extracted.Particles above a defined particle size are sieved off by the sievingdevice 1105 and removed through the discharge 1107. The sievepermeability of the sieving device 1105 can be selected to correspond tothe particle size to be sieved off. The remaining particles, a silicondioxide granulate having the desired particle size, are removed throughthe outlet 1108.

In FIG. 10 is shown a schematic cross section through a light guide 1200according to the invention which has a core 1201 and a jacket M1 1202which surrounds the core 1201.

FIG. 11 shows schematically a top view of a guide 1300 which has cablestructure. In order to represent the arrangement of the core 1301 andthe jacket M1 1302 around the core 1301, a part of the core 1301 isshown without the jacket M1 1302. Typically however, the core 1301 issheathed over its entire length by the jacket M1 1302.

FIG. 12 shows a preferred embodiment of a crucible 1400. The cruciblehas a solids inlet 1401 and an outlet 1402. In operation, silicondioxide granulate 1403 is present in a reposing cone 1404 in the upperregion of the crucible 1400, whilst a glass melt 1405 is present in thelower region of the crucible. The crucible 1400 has a gas inlet 1406 anda gas outlet 1407. The gas inlet 1406 and the gas outlet 1407 arearranged above the reposing cone 1404 of the silicon dioxide granulate1403. The gas outlet 1406 comprises a pipeline for the gas feed 1408 anda device 1409 for measuring the dew point of the exiting gas. The device1409 comprises a dew point mirror hygrometer (not shown here). Theseparation between the crucible and the device 1409 for measuring thedew point can vary. A quartz glass body 1410 can be removed through theoutlet 1402 of the crucible 1400.

FIG. 13 shows a preferred embodiment of the oven 1500 which is suitablefor a vacuum sintering process, a gas pressure sinter process and inparticular a combination thereof. The oven has from outside inward apressure resistant jacket 1501 and a thermal insulating layer 1502. Thespace enclosed thereby, referred to as the oven interior, can be chargedwith a gas or a gas mixture via a gas feed 1504. Further, the oveninterior has a gas outlet 1505 via which gas can be removed. Accordingto the gas transport balance between gas feed 1504 and gas removal at1505 an over pressure, a vacuum or also a gas flow can be produced inthe interior of the oven 1500. Further, heating elements 1506 arepresent in the oven interior 1500. These are often mounted on theinsulation layer 1502 (not shown here). For protecting the melt materialfrom contamination, there is a so-called “liner” 1507 in the interior ofthe oven, which separates the oven chamber 1503 from the heatingelements 1506. Moulds 1508 with material to be melted 1509 can beintroduced into the oven chamber 1503. The mould 1508 can be open on aside (shown here) or can completely enclose the melt material 1509 (notshown).

FIG. 14 shows a flow diagram containing the steps 1601 and 1602 of aprocess for the preparation of a formed body. In the first step 1601, aquartz glass body is provided, preferably a quartz glass body preparedaccording to process 100. Such a quartz glass body can be a solid orhollow body quartz glass body. In a second step 1602, a formed body isformed from a solid quartz glass body provided in step 1601.

Test Methods

a. Fictive Temperature

The fictive temperature is measured by Raman spectroscopy using theRaman scattering intensity at about 606 cm⁻¹. The procedure and analysisdescribed in the contribution of Pfleiderer et. al.; “The UV-induced 210nm absorption band in fused Silica with different thermal history andstoichiometry”; Journal of Non-Crystalline Solids, volume 159 (1993),pages 145-153.

b. OH Content

The OH content of the glass is measured by infrared spectroscopy. Themethod of D. M. Dodd & D. M. Fraser “Optical Determinations of OH inFused Silica” (J.A.P. 37, 3991 (1966)) is employed. Instead of thedevice named therein, an FTIR-spectrometer (Fourier transform infraredspectrometer, current System 2000 of Perkin Elmer) is employed. Theanalysis of the spectra can in principle be performed on either theabsorption band at ca. 3670 cm⁻¹ or on the absorption band at ca. 7200cm⁻¹. The selection of the band is made on the basis that thetransmission loss through OH absorption is between 10 and 90%.

c. Oxygen Deficiency Centers (ODCs)

For the quantitative detection, the ODC(I) absorption is measured at 165nm by means of a transmission measurement at a probe with thicknessbetween 1-2 mm using a vacuum UV spectrometer, model VUVAS 2000, ofMcPherson, Inc. (USA).

Then:

N=α/σ

with

-   -   N=defect concentration [1/cm³]    -   α=optical absorption [1/cm, base e] of the ODC(I) band

σ=effective cross section [cm²]

wherein the effective cross section is set to σ=7.5·10⁻¹⁷ cm² (from L.Skuja, “Color Centers and Their Transformations in Glassy SiO₂”,Lectures of the summer school “Photosensitivity in optical Waveguidesand glasses”, Jul. 13-18 1998, Vitznau, Switzerland).

d. Elemental Analysis

d-1) Solid samples are crushed. Then, ca. 20 g of the sample is cleanedby introducing it into a HF-resistant vessel fully, covering it with HFand thermally treating at 100° C. for an hour. After cooling, the acidis discarded and the sample cleaned several times with high puritywater. Then, the vessel and the sample are dried in the drying cabinet.

Next, ca. 2 g of the solid sample (crushed material cleaned as above;dusts etc. without pretreatment) is weighed into an HF resistantextraction vessel and dissolved in 15 ml HF (50 wt.-%). The extractionvessel is closed and thermally treated at 100° C. until the sample iscompletely dissolved. Then, the extraction vessel is opened and furtherthermally treated at 100° C., until the solution is completelyevaporated. Meanwhile, the extraction vessel is filled 3× with 15 ml ofhigh purity water. 1 ml HNO₃ is introduced into the extraction vessel,in order to dissolve separated impurities and filled up to 15 ml withhigh purity water. The sample solution is then ready.

d-2) ICP-MS/ICP-OES Measurement

Whether OES or MS is employed depends on the expected elementalconcentrations. Typically, measurements of MS are 1 ppb, and for OESthey are 10 ppb (in each case based on the weighed sample). Themeasurement of the elemental concentration with the measuring device isperformed according to the stipulations of the device manufacturer(ICP-MS: Agilent 7500ce; ICP-OES: Perkin Elmer 7300 DV) and usingcertified reference liquids for calibration. The elementalconcentrations in the solution (15 ml) measured by the device are thenconverted based on the original weight of the probe (2 g).

Note: It is to be kept in mind that the acid, the vessels, the water andthe devices must be sufficiently pure in order to measure the elementalconcentrations in question. This is checked by extracting a blank samplewithout quartz glass.

The following elements are measured in this way: Li, Na, Mg, K, Ca, Fe,Ni, Cr, Hf, Zr, Ti, (Ta), V, Nb, W, Mo, Al.

d-3) The measurement of samples present as a liquid is carried out asdescribed above, wherein the sample preparation according to step d-1)is skipped. 15 ml of the liquid sample are introduced into theextraction flask. No conversion based on the original sample weight ismade.

e. Determination of Density of a Liquid

For measuring the density of a liquid, a precisely defined volume of theliquid is weighed into a measuring device which is inert to the liquidand its constituents, wherein the empty weight and the filled weight ofthe vessel are measured. The density is given as the difference betweenthe two weight measurements divided by the volume of the liquidintroduced.

f Fluoride Determination

15 g of a quartz glass sample is crushed and cleaned by treating innitric acid at 70° C. The sample is then washed several times with highpurity water and then dried. 2 g of the sample is weighed into a nickelcrucible and covered with 10 g Na₂CO₃ and 0.5 g ZnO. The crucible isclosed with a Ni-lid and roasted at 1000° C. for an hour. The nickelcrucible is then filled with water and boiled up until the melt cake hasdissolved entirely. The solution is transferred to a 200 ml measuringflask and filled up to 200 ml with high purity water. Aftersedimentation of undissolved constituents, 30 ml are taken andtransferred to a 100 ml measuring flask, 0.75 ml of glacial acetic acidand 60 ml TISAB are added and filled up with high purity water. Thesample solution is transferred to a 150 ml glass beaker.

The measurement of the fluoride content in the sample solution isperformed by means of an ion sensitive (fluoride) electrode, suitablefor the expected concentration range, and display device as stipulatedby the manufacturer, here a fluoride ion selective electrode andreference electrode F-500 with R503/D connected to a pMX 3000/pH/IONfrom WissenschaftlichTechnische Werkstatten GmbH. With the fluorideconcentration in the solution, the dilution factor and the sampleweight, the fluoride concentration in the quartz glass is calculated.

g. Determination of Chlorine (>=50 ppm)

15 g of a quartz glass sample is crushed and cleaned by treating withnitric acid at ca. 70° C. Subsequently, the sample is rinsed severaltimes with high purity water and then dried. 2 g of the sample are thenfilled into a PTFE-insert for a pressure container, dissolved with 15 mlNaOH (c=10 mol/l), closed with a PTFE lid and placed in the pressurecontainer. It is closed and thermally treated at ca. 155° C. for 24hours. After cooling, the PTFE insert is removed and the solution istransferred entirely to a 100 ml measuring flask. There, 10 ml HNO₃ (65wt.-%) and 15 ml acetate buffer and added, allowed to cool and filled to100 ml with high purity water. The sample solution is transferred to a150 ml glass beaker. The sample solution has a pH value in the rangebetween 5 and 7.

The measurement of the chloride content in the sample solution isperformed by means of an ion sensitive (Chloride) electrode which issuitable for the expected concentration range, and a display device asstipulated by the manufacturer, here an electrode of type C1-500 and areference electrode of type R-503/D attached to a pMX 3000/pH/ION fromWissenschaftlichTechnische Werkstatten GmbH.

h. Chlorine Content (<50 ppm)

Chlorine content <50 ppm up to 0.1 ppm in quartz glass is measured byneutron activation analysis (NAA). For this, 3 bores, each of 3 mmdiameter and 1 cm long are taken from the quartz glass body underinvestigation. These are given to a research institute for analysis, inthis case to the institute for nuclear chemistry of theJohannes-Gutenberg University in Mainz, Germany. In order to excludecontamination of the sample with chlorine, a thorough cleaning of thesample in an HF bath on location directly before the measurement wasarranged. Each bore is measured several times. The results and the boresare then sent back by the research institute.

i. Optical Properties

The transmission of quartz glass samples is measured with the commercialgrating- or FTIR-spectrometer from Perkin Elmer (Lambda 900 [190-3000nm] or System 2000 [1000-5000 nm]). The selection is determined by therequired measuring range.

For measuring the absolute transmission, the sample bodies are polishedon parallel planes (surface roughness RMS <0.5 nm) and the surface iscleared off all residues by ultrasound treatment. The sample thicknessis 1 cm. In the case of an expected strong transmission loss due toimpurities, dopants etc., a thicker or thinner sample can be selected inorder to stay within the measuring range of the device. A samplethickness (measuring length) is selected at which only slight artefactsare produced on account of the passage of the radiation through thesample and at the same time a sufficiently detectable effect ismeasured.

The measurement of the opacity, the sample is placed in front of anintegrating sphere. The opacity is calculated using the measuredtransmission value T according to the formula: 0=1/T=I₀/I.

j. Refractive Index and Distribution of Refractive Index in a Tube orRod

The distribution of refractive index of tubes/rods can be characterisedby means of a York Technology Ltd. Preform Profiler P102 or P104. Forthis, the rod is placed lying in the measuring chamber the chamber isclosed tight. The measuring chamber is then filled with an immersion oilwhich has a refractive index at the test wavelength of 633 nm, which isvery similar to that of the outermost glass layer at 633 nm. The laserbeam then goes through the measuring chamber. Behind the measuringchamber (in the direction of the of the radiation) is mounted a detectorwhich measures the angle of deviation (of the radiation entering themeasuring chamber compared to the radiation exiting the measuringchamber). Under the assumption of radial symmetry of the distribution ofrefractive index of the rod, the diametral distribution of refractiveindex can be reconstructed by means of an inverse Abel transformation.These calculations are performed by the software of the devicemanufacturer York.

The refractive index of a sample is measured with the York TechnologyLtd. Preform Profiler P104 analogue to the above description. In thecase of isotropic samples, measurement of distribution of refractiveindex gives only one value, the refractive index.

k. Carbon Content

The quantitative measurement of the surface carbon content of silicondioxide granulate and silicon dioxide powder is performed with a carbonanalyser RC612 from Leco Corporation, USA, by the complete oxidation ofall surface carbon contamination (apart from SiC) with oxygen to obtaincarbon dioxide. For this, 4.0 g of a sample are weighed and introducedinto the carbon analyser in a quartz glass dish. The sample is bathed inpure oxygen and heated for 180 seconds to 900° C. The CO₂ which forms ismeasured by the infrared detector of the carbon analyser. Under thesemeasuring conditions, the detection limit lies at <1 ppm (weight-ppm)carbon.

A quartz glass boat which is suitable for this analysis using the abovenamed carbon analyser is obtainable as a consumable for the LECOanalyser with LECO number 781-335 on the laboratory supplies market, inthe present case from Deslis Laborhandel, FlurstraBe 21, D40235Dusseldorf (Germany), Deslis-No. LQ-130XL. Such a boat haswidth/length/height dimensions of ca. 25 mm/60 mm/15 mm. The quartzglass boat is filled up to half its height with sample material. Forsilicon dioxide powder, a sample weight of 1.0 g sample material can bereached. The lower detection limit is then <1 weight ppm carbon. In thesame boat, a sample weight of 4 g of a silicon dioxide granulate isreached for the same filling height (mean particle size in the rangefrom 100 to 500 μm). The lower detection limit is then about 0.1 weightppm carbon. The lower detection limit is reached when the measurementsurface integral of the sample is not greater than three times themeasurement surface integral of an empty sample (empty sample=the aboveprocess but with an empty quartz glass boat).

l. Curl Parameter

The curl parameter (also called: “Fibre Curl”) is measured according toDIN EN 60793-1-34:2007-01 (German version of the standard IEC60793-1-34:2006). The measurement is made according to the methoddescribed in Annex A in the sections A.2.1, A.3.2 and A.4.1 (“extrematechnique”).

m. Attenuation

The attenuation is measured according to DIN EN 60793-1-40:2001 (Germanversion of the standard IEC 60793-1-40:2001). The measurement is madeaccording to the method described in the annex (“cut-back method”) at awavelength of λ=1550 nm.

n. Viscosity of the Slurry

The slurry is set to a concentration of 30 weight-% solids content withdemineralised water (Direct-Q 3UV, Millipore, Water quality: 18.2 MΩcm). The viscosity is then measured with a MCR102 from Anton-Paar. Forthis, the viscosity is measured at 5 rpm. The measurement is made at atemperature of 23° C. and an air pressure of 1013 hPa.

o. Thixotropy

The concentration of the slurry is set to a concentration of 30 weight-%of solids with demineralised water (Direct-Q 3UV, Millipore, waterquality: 18.2 MΩ cm). The thixotropy is then measured with an MCR102from Anton-Paar with a cone and plate arrangement. The viscosity ismeasured at 5 rpm and at 50 rpm. The quotient of the first and thesecond value gives the thixotropic index. The measurement is made at atemperature of 23° C.

p. Zeta Potential of the Slurry

For zeta potential measurements, a zeta potential cell (Flow Cell,Beckman Coulter) is employed. The sample is dissolved in demineralisedwater (Direct-Q 3UV, Millipore, water quality: 18.2 MΩ cm) to obtain a20 mL solution with a concentration of 1 g/L. The pH is set to 7 throughaddition of HNO₃ solutions with concentrations of 0.1 mol/L and 1 mol/Land an NaOH solution with a concentration of 0.1 mol/L. The measurementis made at a temperature of 23° C.

q. Isoelectric Point of the Slurry

The isoelectric point, a zeta potential measurement cell (Flow Cell,Beckman Coulter) and an auto titrator (DelsaNano AT, Beckman Coulter) isemployed. The sample is dissolved in demineralised water (Direct-Q 3UV,Millipore, water quality: 18.2 MΩ cm) to obtain a 20 mL solution with aconcentration of 1 g/L. The pH is varied by adding HNO₃ solutions withconcentrations of 0.1 mol/L and 1 mol/L and an NaOH solution with aconcentration of 0.1 mol/L. The isoelectric point is the pH value atwhich the zeta potential is equal to 0. The measurement is made at atemperature of 23° C.

r. pH Value of the Slurry

The pH value of the slurry is measured using a WTW 3210 fromWissenschaftlich-Technische-Werkstatten GmbH. The pH 3210 Set 3 from WTWis employed as electrode. The measurement is made at a temperature of23° C.

s. Solids content

A weighed portion m₁ of a sample is heated for 4 hours to 500° C.reweighed after cooling (m₂). The solids content w is given as m₂/m₁*100[Wt. %].

t. Bulk Density

The bulk density is measured according to the standard DIN ISO697:1984-01 with an SMG 697 from Powtec. The bulk material (silicondioxide powder or granulate) does not clump.

u. Tamped Density (Granulate)

The tamped density is measured according to the standard DIN ISO787:1995-10.

v. Measurement of the Pore Size Distribution

The pore size distribution is measured according to DIN 66133 (with asurface tension of 480 mN/m and a contact angle of 140°). For themeasurement of pore sizes smaller than 3.7 nm, the Pascal 400 fromPorotec is used. For the measurement of pore sizes from 3.7 nm to 100μm, the Pascal 140 from Porotec is used. The sample is subjected to apressure treatment prior to the measurement. For this a manual hydraulicpress is used (Order-No. 15011 from Specac Ltd., River House, 97 CrayAvenue, Orpington, Kent BR5 4HE, U.K.). 250 mg of sample material isweighed into a pellet die with 13 mm inner diameter from Specac Ltd. andloaded with 1 t, as per the display. This load is maintained for 5 s andreadjusted if necessary. The load on the sample is then released and thesample is dried for 4 h at 105±2° C. in a recirculating air dryingcabinet.

The sample is weighed into the penetrometer of type 10 with an accuracyof 0.001 g and in order to give a good reproducibility of themeasurement it is selected such that the stem volume used, i.e. thepercentage of potentially used Hg volume for filling the penetrometer isin the range between 20% to 40% of the total Hg volume. The penetrometeris then slowly evacuated to 50 μm Hg and left at this pressure for 5min. The following parameters are provided directly by the software ofthe measuring device: total pore volume, total pore surface area(assuming cylindrical pores), average pore radius, modal pore radius(most frequently occurring pore radius), peak n. 2 pore radius (μm).

w. Primary Particle Size

The primary particle size is measured using a scanning electronmicroscope (SEM) model Zeiss Ultra 55. The sample is suspended indemineralised water (Direct-Q 3UV, Millipore, water quality: 18.2 MΩcm), to obtain an extremely dilute suspension. The suspension is treatedfor 1 min with the ultrasound probe (UW 2070, Bandelin electronic, 70 W,20 kHz) and then applied to a carbon adhesive pad.

x. Mean Particle Size in Suspension

The mean particle size in suspension is measured using a Mastersizer2000, available from Malvern Instruments Ltd., UK, according to the usermanual, using the laser deflection method. The sample is suspended indemineralised water (Direct-Q 3UV, Millipore, water quality: 18.2 MΩ cm)to obtain a 20 mL suspension with a concentration of 1 g/L. Thesuspension is treated with the ultrasound probe (UW 2070, Bandelinelectronic, 70 W, 20 kHz) for 1 min.

y. Particle Size and Core Size of the Solid

The particle size and core size of the solid are measured using aCamsizer XT, available from Retsch Technology GmbH, Deutschlandaccording to the user manual. The software gives the D10, D50 and D90values for a sample.

z. BET Measurement

For the measurement of the specific surface area, the static volumetricBET method according to DIN ISO 9277:2010 is used. For the BETmeasurement, a “NOVA 3000” or a “Quadrasorb” (available fromQuantachrome), which operate according to the SMART method (“SorptionMethod with Adaptive dosing Rate”), is used. The micropore analysis isperformed using the t-plot process (p/p0=0.1-0.3) and the mesoporeanalysis is performed using the MBET process (p/p0=0.0-0.3). Asreference material, the standards alumina SARM-13 and SARM-214,available from Quantachrome are used. The tare weight of the measuringcell (clean and dry) is weighed. The type of measuring cell is selectedsuch that the sample material which is introduced and the filler rodfill the measuring cell as much as possible and the dead space isreduced to a minimum. The sample material is introduced into themeasuring cell. The amount of sample material is selected so that theexpected value of the measurement value corresponds to 10-20 m²/g. Themeasuring cells are fixed in the baking positions of the BET measuringdevice (without filler rod) and evacuated to <200 mbar. The speed of theevacuation is set so that no material leaks from the measuring cell.Baking is performed in this state at 200° C. for 1 h. After cooling, themeasuring cell filled with the sample is weighed (raw value). The tareweight is then subtracted from the raw value of the weight=nettweight=weight of the sample. The filling rod is then introduced into themeasuring cell this is again fixed at the measuring location of the BETmeasuring device. Prior to the start of the measurement, the sampleidentifications and the sample weights are entered into the software.The measurement is started. The saturation pressure of nitrogen gas (N24.0) is measured. The measuring cell is evacuated and cooled down to 77K using a nitrogen bath. The dead space is measured using helium gas (He4.6). The measuring cell is evacuated again. A multi-point analysis withat least 5 measuring points is performed. N2 4.0 is used as absorptive.The specific surface area is given in m²/g.

za. Viscosity of Glass Bodies

The viscosity of the glass is measured using the beam bendingviscosimeter of type 401 from TA Instruments with the manufacturer'ssoftware WinTA (current version 9.0) in Windows 10 according to the DINISO 7884-4:1998-02 standard. The support width between the supports is45 mm. Sample rods with rectangular cross section are cut from regionsof homogeneous material (top and bottom sides of the sample have afinish of at least 1000 grain). The sample surfaces after processinghave a grain size=9 μm & RA=0.15 μm. The sample rods have the followingdimensions: length=50 mm, width=5 mm & height=3 mm (ordered: length,width, height, as in the standards document). Three samples are measuredand the mean is calculated. The sample temperature is measured using athermocouple tight against the sample surface. The following parametersare used: heating rate=25 K up to a maximum of 1500° C., loadingweight=100 g, maximum bending=3000 μm (deviation from the standardsdocument).

zb. Dew Point Measurement

The dew point is measured using a dew point mirror hygrometer called“Optidew” of the company Michell Instruments GmbH, D-61381Friedrichsdorf. The measuring cell of the dew point mirror hygrometer isarranged at a distance of 100 cm from the gas outlet of the oven.

For this, the measuring device with the measuring cell is connected ingas communication to the gas outlet of the oven via a T-piece and a hose(Swagelok PFA, Outer diameter: 6 mm). The over pressure at the measuringcell is 10±2 mbar. The through flow of the gas through the measuringcell is 1-2 standard litre/min. The measuring cell is in a room with atemperature of 25° C., 30% relative air humidity and a mean pressure of1013 hPa.

zc. Residual Moisture (Water Content)

The measurement of the residual moisture of a sample of silicon dioxidegranulate is performed using a Moisture Analyzer HX204 from MettlerToledo. The device functions using the principle of thermogravimetry.The HX204 is equipped with a halogen light source as heating element.The drying temperature is 220° C. The starting weight of the sample is10 g±10%. The “Standard” measuring method is selected. The drying iscarried out until the weight change reaches not more than 1 mg/140 s.The residual moisture is given as the difference between the initialweight of the sample and the final weight of the sample, divided by theinitial weight of the sample.

The measurement of residual moisture of silicon dioxide powder isperformed according to DIN EN ISO 787-2:1995 (2 h, 105° C.).

Examples

The example is further illustrated in the following through examples.The invention is not limited by the examples.

A. 1. Preparation of Silicon Dioxide Powder (OMCTS Route)

An aerosol formed by atomising a siloxane with air (A) is introducedunder pressure into a flame which is formed by igniting a mixture ofoxygen enriched air (B) and hydrogen. Furthermore, a gas flow (C)surrounding the flame is introduced and the process mixture is thencooled with process gas. The product is separated off at a filter. Theprocess parameters are given in Table 1 and the specifications of theresulting product are given in Table 2. Experimental data for thisexample are indicated with A1-x.

2. Modification 1: Increased Carbon Content

A process was carried out as described in A.1., but the burning of thesiloxane was performed in such a way that an amount of carbon was alsoformed. Experimental data for this example are indicated with A2-x.

TABLE 1 Example A1-1 A2-1 A2-2 Aerosol formation Siloxane OMCTS* OMCTS*OMCTS* Feed rate kg/h 10 10 10 (kmol/h) (0.0337) (0.0337) (0.0337) Feedrate of air (A) Nm³/h 14 10 12 Pressure barO 1.2 1.2 1.2 Burner feedOxygen enriched air (B) Nm³/h 69 65 68 O₂-content Vol. % 32 30 32 TotalO₂ feed rate Nm³/h 25.3 21.6 24.3 kmol/h 1.130 0.964 1.083 Hydrogen feedrate Nm³/h 27 27 12 kmol/h 1.205 1.205 0.536 Feed — — Carbon compoundMaterial methane Amount Nm³/h 5.5 Air flow (C) Nm³/h 60 60 60Stoichiometric ratio V 2.099 1.789 2.011 X 0.938 0.80 2.023 Y 0.9910.845 0.835 V = molar ratio of employed O₂/O₂ required for completedoxidation of the siloxane; X = molar ratio O₂/H₂; Y = (molar ratio ofemployed O₂/O₂ required for stoichiometric conversion OMCTS + fuel gas);barO = over pressure; *OMCTS = Octamethylcyclotetrasiloxane.

TABLE 2 Example A1-1 A2-1 A2-2 BET m²/g 30 33 34 Bulk density g/ml 0.114+− 0.105 +− 0.103 +− 0.011 0.011 0.011 Tamped density g/ml 0.192 +−0.178 +− 0.175 +− 0.015 0.015 0.015 Primary particle size nm 94 82 78particle size distribution D10 μm 3.978 ± 5.137 ± 4.973 ± 0.380 0.5200.455 particle size distribution D50 μm 9.383 ± 9.561 ± 9.423 ± 0.6860.690 0.662 particle size distribution D90 μm 25.622 ± 17.362 ± 18.722 ±1.387 0.921 1.218 C content ppm 34 ± 4 73 ± 6 80 ± 6 Cl content ppm <60<60 <60 Al content ppb 20 20 20 Total content of metals ppb <700 <700<700 other than Al Residual moisture content wt.-% 0.02-1.0 0.02-1.00.02-1.0 pH value in water 4% (IEP) — 4.8 4.6 4.5 Viscosity at 5 rpm,aqueous mPas 753 1262 1380 suspension 30 wt.-%, 23° C. Alkali earthmetal content ppb 538 487 472

B. 1. Preparation of Silicon Dioxide Powder (Silicon Source: SiCl₄)

A portion of silicon tetrachloride (SiCl₄) is evaporated at atemperature T and introduced with a pressure P into a flame of a burnerwhich is formed by igniting a mixture of oxygen enriched air andhydrogen. The mean normalised gas flow to the outlet is held constant.The process mixture is then cooled with process gas. The product wasseparated off at a filter.

The process parameters are given in Table 3 and the specifications ofthe resulting products are given in Table 4. They are indicated withB1-x.

2. Modification 1: Increased Carbon Content

A process was carried out as described in B.1., but the burning of thesilicon tetrachloride was performed such that an amount of carbon wasalso formed. Experimental data for this example are indicated with B2-x.

TABLE 3 Example B1-1 B2-1 Aerosol formation Silicon tetrachloride kg/h50 50 feed (kmol) (0.294) (0.294) Temperature T ° C. 90 90 Pressure pbarO 1.2 1.2 Burner feed Oxygen enriched air, Nm³/h 145 115 O₂ contenttherein Vol. % 45 30 Feed — Carbon compound Material methane AmountNm³/h 2.0 Hydrogen feed Nm³/h 115 60 kmol/h 5.13 2.678 Stoichiometricratios X 0.567 0.575 Y 0.946 0.85 X = as molar ratio O₂/H₂; Y = molarratio of employed O₂/O₂ required for stoichio-metric reaction withSiCl4+ H2 + CH4); barO = Over pressure.

TABLE 4 Example B1-1 B2-1 BET m²/g 49 47 Bulk density g/ml 0.07 ± 0.010.06 ± 0.01 tamped density g/ml 0.11 ± 0.01 0.10 ± 0.01 Primary particlesize nm 48 43 particle size distribution D10 μm 5.0 ± 0.5 4.5 ± 0.5particle size distribution D50 μm 9.3 ± 0.6 8.7 ± 0.6 particle sizedistribution D90 μm 16.4 ± 0.5  15.8 ± 0.7  C content ppm <4 76 Clcontent ppm 280 330 Al content ppb 20 20 Total of the concentrations ofCa, ppb <1300 <1300 Co, Cr, Cu, Fe, Ge, Hf, K, Li, Mg, Mn, Mo, Na, Nb,Ni, Ti, V, W, Zn, Zr residual moisture content wt.-% 0.02-1.0  0.02-1.0 pH value in water 4% (IEP) pH 3.8 3.8 Viscosity at 5 rpm, aqueous sus-mPas 5653 6012 pension 30 wt.-%, 23° C. Alkali earth metal content ppb550 342

C. Steam Treatment

A particle flow of silicon dioxide powder is introduced via the top of astanding column. Steam at a temperature (A) and air are fed via thebottom of the column. The column is maintained at a temperature (B) atthe top of the column and at a second temperature (C) at the bottom ofthe column by an internally situated heater. After leaving the column(holding time (D)) the silicon dioxide powder has in particular theproperties shown in Table 6. The process parameters are given in Table5.

TABLE 5 Example C-1 C-2 Educt: Product of B1-1 B2-1 Educt feed kg/h 100100 Steam feed kg/h 5 5 Steam temperature (A) ° C. 120 120 Air feedNm³/h 4.5 4.5 Column height m 2 2 Inner diameter mm 600 600 T (B) ° C.260 260 T (C) ° C. 425 425 Holding time (D) silicon s 10 10 dioxidepowder

TABLE 6 Example C-1 C-2 pH value in water 4% (IEP) — 4.6 4.6 Cl contentppm <60 <60 C content ppm <4 36 Viscosity at 5 rpm, aqueous mPas 15231478 suspension 30 wt.-%, 23° C.

The silicon dioxide powders obtained in the examples C-1 and C-2 eachhave a low chlorine content as well as a moderate pH value insuspension. The carbon content of example C-2 is higher as for C-1.

D. Treatment with a Neutralising Agent

A particle flow of silicon dioxide powder is introduced via the top of astanding column. A neutralising agent and air are fed via the bottom ofthe column. The column is maintained at a temperature (B) at the top ofthe column and at a second temperature (C) at the bottom of the columnby an internally situated heater. After leaving the column (holding time(D)) the silicon dioxide powder has in particular the properties shownin Table 8. The process parameters are given in Table 7.

TABLE 7 Example D-1 Educt: Product from B1-1 Educt feed kg/h 100Neutralising agent Ammonia Neutralising agent feed kg/h  1.5Neutralising agent specifications Obtainable from Air Liquide: AmmoniaN38, purity ≥99.98 Vol. % Air feed Nm³/h  4.5 Column height m  2 innerdiameter mm 600 T (B) ° C. 200 T (C) ° C. 250 Holding time (D) ofsilicon s  10 dioxide powder

TABLE 8 Example D-1 pH value in water 4% (IEP) — 4.8 Cl content ppm 210C content ppm <4 Viscosity at 5 rpm, aqueous sus- mPas 821 pension 30wt.-%, 23° C.

E. 1. Preparation of Silicon Dioxide Granulate from Silicon DioxidePowder

A silicon dioxide powder is dispersed in fully desalinated water. Forthis, an intensive mixer of type R from the Gustav Eirich machinefactory is used. The resulting suspension is pumped with a membrane pumpand thereby pressurised and converted into droplets by a nozzle. Theseare dried in a spray tower and collect on the floor of the tower. Theprocess parameters are given in Table 9 and the properties of theobtained granulate in Table 10. Experimental data for this example areindicated with E1-x.

2. Modification 1: Increased Carbon Content

The process is analogous to that described in E.1. Additionally, carbonpowder is dispersed into the suspension. Experimental data for theseexamples are indicated with E2-x.

3. Modification 2: Addition of Silicon

The process is analogous to that described in E.1. Additionally, asilicon component is dispersed into the suspension. Experimental datafor these examples are identified with E3-1.

TABLE 9 Example E1-1 E1-2 E1-3 E1-4 E1-5 E2-1 E3-1 E3-2 E7-11 E7-12E7-13 E7-14 Educt = Product from A1-1 A2-1 B1-1 C-1 C-2 A1-1 A1-1 A2-1A1-1 A1-1 B1-1 B1-1 Amount of educt Kg 10 10 10 10 10 10 10 10 10 10 1010 Carbon powder Material C** Max. Particle size — — — — — 75 — — — — —— Amount μm Silicon component Material — — — — — — sili- — conpul-ver*** Grain size (d50) 8 μm Amount 1000 Carbon content ppm 0.5 ppmTotal of the 5 ppm concentrations of Ca, Co, Cr, Cu, Fe, Ge, Hf, K, Li,Mg, Mn, Mo, Na, Nb, Ni, Ti, V, W, Zn, Zr Water Rating* FD FD FD FD FD FDFD FD FD FD FD FD Liter 5.4 5.4 5.4 5.4 5.4 5.4 5.4 5.4 5.4 5.4 5.4 5.4Dispersion Wt. 65 65 65 65 65 65 65 65 65 65 65 65 Solids content %Nozzle Diameter mm 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2Temperature ° C. 25 25 25 25 25 25 25 25 25 25 25 25 Pressure Bar 16 1616 16 16 16 16 16 16 16 16 16 Installation height m 6.5 6.5 6.5 6.5 6.56.5 6.5 6.5 6.5 6.5 6.5 6.5 Spray tower Height m 18.20 18.20 18.20 18.2018.20 18.20 18.20 18.20 18.20 18.20 18.20 18.20 Inner diameter m 6.306.30 6.30 6.30 6.30 6.30 6.30 6.30 6.30 6.30 6.30 6.30 T (introducedgas) ° C. 380 380 380 380 380 380 380 380 380 380 380 380 T (exhaust) °C. 110 110 110 110 110 110 110 110 110 110 110 1110 Air flow m³/h 65006500 6500 6500 6500 6500 6500 6500 6500 6500 6500 6500 Installationheight = distance between nozzle and lowest point of the spray towerinterior in the direction of gravity. *FD = fully desalinated,conductance ≤0.1 μS; **C 006011: Graphite powder, max. particle size: 75μm, high purity (available from Goodfellow GmbH, Bad Nauheim (Germany);***available from Wacker Chemie AG (Munich, Germany).

TABLE 10 Example E1-1 E1-2 E1-3 E1-4 E1-5 E2-1 E3-1 E3-2 E7-11 E7-12E7-13 E7-14 BET m²/g 30  33 49 49 47 28 31 35 31 32 50 53 Bulk densityg/ml 0.8 ± 0.8 ± 0.8 ± 0.8 ± 0.8 ± 0.8 ± 0.8 ± 0.8 ± 0.8 ± 0.8 ± 0.8 ±0.8 ± 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 tamped den- g/ml0.9 ± 0.9 ± 0.9 ± 0.9 ± 0.9 ± 0.9 ± 0.9 ± 0.9 ± 0.9 ± 0.9 ± 0.9 ± 0.9 ±sity 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 mean particle sizeμm 255 255 255 255 255 255 255 255 255 255 255 255 particle size μm 110110 110 110 110 110 110 110 110 110 110 110 distribution D10 particlesize μm 222 222 222 222 222 222 222 222 222 222 222 222 distribution D50particle size μm 390 390 390 390 390 390 390 390 390 390 390 390distribution D90 SPHT3 Dim- 0.64- 0.64- 0.64- 0.64- 0.64- 0.64- 0.64-0.64- 0.64- 0.64- 0.64- 0.64- less 0.98 0.98 0.98 0.98 0.98 0.98 0.980.98 0.98 0.98 0.98 0.98 Aspect ratio Dim- 0.64- 0.64- 0.64- 0.64- 0.64-0.64- 0.64- 0.64- 0.64- 0.64- 0.64- 0.64- W/L (width to less 0.94 0.940.94 0.94 0.94 0.94 0.94 0.94 0.94 0.94 0.94 0.94 length) C content ppm<4 39 <4 <4 32 100 <4 39 <4 <4 <4 <4 Cl content ppm <60 <60 280 <60 <60<60 <60 <60 <60 <60 <280 <280 Al content ppb 20 20 20 20 20 20 20 20 2020 20 20 Total of the ppb <700 <1300 <1300 <1300 <700 <700 <700 <700<700 <700 <700 <700 concentrations of Ca, Co, Cr, Cu, Fe, Ge, Hf, K, Li,Mg, Mn, Mo, Na, Nb, Ni, Ti, V, W, Zn, Zr residual moisture wt.-% <3 <3<3 <3 <3 <3 <3 <3 <3 <3 <3 <3 content Alkaline earth ppb 538 487 550 550342 538 538 487 553 482 544 549 metal content Pore volume ml/g 0.33 0.330.45 0.45 0.45 0.33 0.33 0.33 0.33 0.33 0.45 0.45 angle of repose ° 2626 26 26 26 26 26 26 26 26 26 26 The granulates are all open pored, havea uniform and spherical shape (all by microscopic investigation). Theytend not to stick together or cement.

F. Cleaning Silicon Dioxide Granulate

Silicon dioxide granulate is first optionally treated with oxygen ornitrogen (see Table 11) at a temperature T1. Subsequently, the silicondioxide granulate is treated with a co-flow of a chlorine containingcomponent, wherein the temperature is raised to a temperature T2. Theprocess parameters are given in Table 11 and the properties of theobtained treated granulate in Table 12.

TABLE 11 Example F1-1 F1-2 F1-3 F1-4 F1-5 F2-1 F3-1 F3-2 F7-11 F7-12F7-13 F7-14 Educt = E1-1 E1-2 E1-3 E1-4 E1-5 E2-1 E3-1 E3-2 E7-11 E7-12E7-13 E7-14 Product from Rotary kiln ¹⁾ length cm 200 200 200 200 200200 200 200 200 200 Inner dia- cm 10 10 10 10 10 10 10 10 10 10 meterThrough- kg/h 2 2 2 2 2 2 2 2 2 2 put Rotational rpm 2 2 2 2 2 2 2 2 2 2speed Tl ° C. 1100 NA 1100 1100 1100 NA 1100 1100 1100 1100 1100 1100Atmosphere O2 NA O2 O2 O2 NA N2 N2 O₂ O₂ O₂ O₂ pure pure pure pure purepure pure pure Reactant O2 NA O2 O2 O2 NA None None O₂ O₂ O₂ O₂ Feed 300l/h NA 300 l/h 300 l/h 300 l/h NA 300 l/h 300 l/h 300 l/h 300 l/h noneNA None none none NA <1 <1 <1 <1 residual wt.-% <1 <3 <1 <1 <1 <3 <1 <1moisture 1100 1100 1100 1100 content T2 ° C. 1100 1100 1100 1100 11001100 NA NA Co-flow 50 50 50 50 Component 1: 1/h 50 50 50 50 50 50 NA NA0 0 0 0 HCl Component 2: 1/h 0 15 0 0 0 15 NA NA Cl2 1/h 50 35 50 50 5035 NA NA 50 50 50 50 Component 3: N2 Total 1/h 100 100 100 100 100 100NA NA 100 100 100 100 co-flow ¹⁾ For the rotary kilns, the throughput isselected as the control variable. That means that during operation themass flow exiting from the rotary kiln is weighed and then therotational speed and/or the inclination of the rotary kiln is adaptedaccordingly. For example, an increase in the throughput can be achievedby a) increasing the rotational speed, or b) increasing the inclinationof the rotary kiln away from horizontal, or a combination of a) and b).

TABLE 12 Example F1-1 F1-2 F1-3 F1-4 F1-5 F2-1 F3-1 F3-2 F7-11 F7-12F7-13 F7-14 BET m²/g  25  27  43  45  40  23  25  26  26  27  46  47 Ccontent ppm  <4  <4  <4  <4  <4  <4  <4  <4  <4  <4  <4  <4 Cl contentppm 100-200 100-200 300-400 100-200 100-200 100-200 <60 <60 <100 <100300-400 300-400 Al content ppb  20  20  20  20  20  20  20  20  20  20 20  20 Pore volume mm³/g 650 650 650 650 650 650 650 650 650 650 650650 Total of the con- ppb <200   <200   <200   <200   <200   <200  <700   <700   <700   <700   <700   <700   centrations of Ca, Co, Cr, Cu,Fe, Ge, Hf, K, Li, Mg, Mn, Mo, Na, Nb, Ni, Ti, V, W, Zn, Zr Alkalineearth ppb 115  55  95 115  40  35 136  33 121  57  90 102 metal contenttamped density g/cm³ 0.95 ± 0.95 ± 0.95 ± 0.95 ± 0.95 ± 0.95 ± 0.95 ±0.95 ± 0.95 ± 0.95 ± 0.95 ± 0.95 ± 0.05 0.05 0.05 0.05 0.05 0.05 0.050.05 0.05 0.05 0.05 0.05 Angle of repose °  26  26  26  26  26  26  26 26  26  26  26  26 n.d. = not determined In the case of F1-2, F2-1 andF3-2, the granulates after the cleaning step show a significantlyreduced carbon content (like low carbon granulate, e.g. F1). Inparticular, F1-2, F1-5, F2-1 and F3-2 show a significantly reducedcontent of alkaline earth metals. SiC formation was not observed.

G. Treatment of Silicon Dioxide Granulate by Warming

Silicon dioxide granulate is subjected to a temperature treatment in apre chamber in the form of a rotary kiln which is positioned upstream ofthe melting oven and which is connected in flow connection to themelting oven via a further intermediate chamber. The rotary kiln ischaracterised by a temperature profile which increases in the flowdirection. A further treated silicon dioxide granulate was obtained. Inexample G-4-2 no treatment by warming was performed during mixing in therotary kiln. The process parameters are given in Table 13 and theproperties of the obtained treated granulate in Table 14.

In all cases except G/H 7-12 and G/H 7-14, the rotary kiln is inmaterial communication with melting oven. IN case G7-12 and G7-14, thegranulate treated in example stage G is removed and taken to a meltingoven, in which the example stage H is then performed.

TABLE 13 Example G1-1 G1-2 G1-3 G1-4 G1-5 G2-1 G3-1 G3-2 G4-1 G4-2 G7-11G7-12 G7-13 G7-14 Educt = Pro- F1-1 F1-2 F1-3 F1-4 F1-5 F2-1 F3-1 F3-2F1-1 F1-1 F7-11 F7-12 F7-13 F7-14 duct from Silicon components Material— — — — — — — — Sili- Sili- — — — — Amount con con pow- pow- der***der*** 0.01% 0.1% Rotary kiln Length cm 200  200  200  200  200  200 200  200  200  NA 200  200  200  200  Inner diameter cm 10 10 10 10 1010 10 10 10 10 10 10 10 Throughput kg/h  8  5  5  5  5  5  5  5  5  5  5 5  5 Rotation speed rpm 30 30 30 30 30 30 30 30 30 30 30 30 30 T1(Rotary ° C. RT RT RT RT RT RT RT RT RT RT RT RT RT kiln inlet) T2(Rotary ° C. 500  500  500  500  500  500  500  500  500  500  500  500 500  kiln outlet) Atmosphere Gas, flow air, O₂, O₂, O₂, O₂, O₂, O₂, O₂,O₂, O₂, O₂, O₂, O₂, direction free in in in in in in in in in in in incon- con- con- con- con- con- con- con- con- count- count- count- count-vec- tra- tra- tra- tra- tra- tra- tra- tra- er er er er tion flow flowflow flow flow flow flow flow flow flow flow flow Total Nm³/   0.6   0.6  0.6   0.6   0.6   0.6   0.6   0.6   0.6   0.6   0.6   0.6 throughput hof gas flow *** Grain size D₅₀ = 8 μm; carbon content ≤ 5 ppm; Totalforeign metals ≤ 5 ppm; 0.5 ppm; available from Wacker Chemie AG (MunichGermany). RT = room temperature ¹⁾ For the rotary kilns, the throughputis selected as the control variable. That means that during operationthe mass flow exiting from the rotary kiln is weighed and then therotational speed and/or the inclination of the rotary kiln is adaptedaccordingly. For example, an increase in the throughput can be achievedby a) increasing the rotational speed, or b) increasing the inclinationof the rotary kiln away from horizontal, or a combination of a) and b).

TABLE 14 Example G1-1 G1-2 Gl-3 Gl-4 Gl-5 G2-1 G3-1 G3-2 G4-1 G4-2 G7-11G7-12 G7-13 G7-14 BET m²/g  22  23  38  42  37  22  22  21  22    24  22 23  42  44 Water content ppm 500 100 100 100 100 100 500 100 500 <10000286 935 533 1512 (residual moisture) C content ppm  <4  <4  <4  <4  <4 <4  <4  <4  <4    <4  <4  <4  <4   <4 Cl content ppm 100- 100- 300-100- 100- 100- <60 <60 100- 100-  84  83 300- 300- 200 200 400 200 200200 200    200 400 400 Al content ppb  20  20  20  20  20  20  20  20 20    20  20  20  20  20 Total of the ppb ≤200    ≤200    ≤200   ≤200  ≤200  ≤200  ≤200   ≤200   ≤200     ≤200 ≤200  ≤200   ≤200   ≤200 concentra- tions of Ca, Co, Cr, Cu, Fe, Ge, Hf, K, Li, Mg, Mn, Mo, Na,Nb, Ni, Ti, V, W, Zn, Zr Alkaline earth ppb 115  55  95 115  40  35 136 33 115    115  21  57 118  115 metalcontent angle of repose °  26  26 26  26  26  26  26  26  26    26  26  26  26  26 Due to this treatment,G3-1 and G3-2 exhibit a significantly reduced alkaline earth metalcontent in comparison to before (E3-1 & E3-2 respectively).

H. Melting of Granulate to Obtain Quartz Glass

Silicon dioxide granulate according to line 2 of Table 15 is employedfor preparing a quartz glass tube in a vertical crucible drawingprocess. The structure of the standing oven, for example H5-1 comprisinga standing melting crucible is shown schematically in FIG. 7, and forall the other examples with a hanging melting crucible FIG. 6 serves asa schematic representation. The silicon dioxide granulate is introducedvia the solids feed and the interior of the melting crucible is flushedwith a gas mixture. In the melting crucible, a glass melt forms uponwhich a reposing cone of silicon dioxide granulate sits. In the lowerregion of the melting crucible, molten glass is removed from the glassmelt through a die (optionally with a mandrel) and is pulled verticallydown in the form of a tubular thread. The output of the plant resultsfrom the weight of the glass melt, the viscosity of the glass throughthe nozzle the size of the hole provided by the nozzle. By varying thefeed rate of silicon dioxide granulate and the temperature, the outputcan be set to the desired level. The process parameters are given inTable 15 and Table 17 and in some cases in Table 19 and the propertiesof the formed quartz glass body in

Table 16 and Table 18.

In Example H7-1, a gas distributing ring is arranged in the meltingcrucible, with which the flushing gas is fed close to the surface of theglass melt. An example of such an arrangement is shown in FIG. 8.

In Example H8-x, the dew point is measured at the gas outlet. Themeasuring principle is shown in FIG. 12. Between the outlet of themelting crucible and the measuring location of the dew point, the gasflow covers a distance of 100 cm.

In all cases except for G/H7-12 and G/H7-14, the rotary kiln is inmaterial communication with the melting oven. In case G7-12 and G7-14,the granulate treated in example stage G was removed and brought to amelting oven in which example stage H was performed.

TABLE 15 Example H1-1 H1-2 H1-3 H1-4 H1-5 H3-1 H3-2 H4-1 H4-2 Educt =Product from G1-1 G1-2 G1-3 G1-4 G1-5 G3-1 G3-2 G4-1 G4-2 Meltingcrucible Type Hanging Hanging Hanging Hanging Hanging Hanging HangingHanging Hanging metal metal metal metal metal metal metal metal metalsheet sheet sheet sheet sheet sheet sheet sheet sheet Type of metal cmcrucible crucible crucible crucible crucible crucible crucible cruciblecrucible Length cm tungsten tungsten tungsten tungsten tungsten tungstentungsten tungsten tungsten Inner diameter 200 150 150 150 150 200 150200 200 40 25 25 25 25 40 25 40 40 Throughput kg/h 30 20 20 20 20 30 2030 30 T1 (Gas compartment of ° C. 300 300 300 300 300 300 300 300 300the melting crucible) T2 (glass melt) ° C. 2100 2100 2100 2100 2100 21002100 2100 2100 T3 (nozzle) ° C. 1900 1900 1900 1900 1900 1900 1900 19001900 Atmosphere/Flushing gas He Vol.-% 50 50 50 50 50 50 50 50 50Concentration H₂ Vol.-% 50 50 50 50 50 50 50 50 50 Concentration Totalgas flow Nm³/h 4 4 4 4 4 2 4 2 2 through-put O₂ ppm ≤100 ≤100 ≤100 ≤100≤100 ≤100 ≤100 ≤100 ≤100

TABLE 16 Example H1-1 H1-2 H1-3 H1-4 H1-5 H3-1 H3-2 H4-1 H4-2 C contentppm <4 <4 <4 <4 <4 <4 <4 <4 <4 Cl content ppm 100-200 100-200 300-400100-200 100-200 <60 <60 100-200 100-200 Al content ppb 20 20 20 20 20 2020 20 20 Total of the con- ppb <400 <400 <400 <400 <400 <400 <400 <400<400 centrations of Ca, Co, Cr, Cu, Fe, Ge, Hf, K, Li, Mg, Mn, Mo, Na,Nb, Ni, Ti, V, W, Zn, Zr OH content ppm 400 400 400 400 400 80 400 80 80Alkaline earth ppb 115 55 95 115 40 136 33 115 115 metal content ODCcontent 1/cm³ 4 * 10¹⁵ 2 * 10¹⁶ 4 * 10¹⁵ 4 * 10¹⁵ 4 * 10¹⁵ 5 * 10¹⁸ 2 *10¹⁶ 5 * 10¹⁸ 8 * 10¹⁸ Pore volume mL/g 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.10.1 Outer diameter cm 19.7 3.0 19.7 19.7 19.7 19.7 3.0 19.7 19.7 tubularthread/ quartz glass body Viscosity Lg(η/ @1250° C. dPas) 12.16 ±12.16 ± 12.16 ± 0.2 0.2 0.2 @1300° C. 11.69 ± 11.69 ± 11.69 ± 11.69 ±11.69 ± 11.49 ± 11.69 ± 11.49 ± 11.49 ± 0.13 0.13 0.13 0.13 0.13 0.150.13 0.15 0.15 @1350° C. 11.26 ± 11.26 ± 11.26 ± 11.26 ± 11.26 ± 10.88 ±11.26 ± 10.88 ± 10.88 ± 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 10.69 ±10.69 ± 10.69 ± 10.69 ± 10.69 ± 10.69 ± 0.07 0.07 0.07 0.07 0.07 0.07“±”-value are the standard deviation.

TABLE 17 Example H5-1 H6-1 H7-1 H8-1 H8-2 H8-3 H8-4 Educt = Product fromG1-1 G1-1 G1-1 G1-1 G1-1 G1-1 G1-1 Melting crucible Type SSt. (W) HSt,(W) HBt, (W) HBt, (W) HBt, (W) HBt, (W) HBt, (W) Type of metal — — Gasdis- TPM TPM TPM TPM tributor ring Additional fittings and fixturesLength cm 250 250 200 200 200 200 200 Inner diameter cm 40 36 40 40 4040 40 Throughput kg/h 40 35 30 30 30 30 30 T1 (Gas com- ° C. 300 400 300300 300 300 300 partment of melting crucible) T2 (glass melt) ° C. 21002150 2100 2100 2100 2100 2100 T3 (Nozzle) ° C. 1900 1900 1900 1900 19001900 1900 Atmosphere He Vol.-% 30 50 50 50 50 50 50 Concentration H₂Vol.-% 70 50 50 50 50 50 50 Concentration Total gas flow Nm³/h 4 4 8 8 43 2 throughput O₂ ppm ≤100 ≤100 ≤10 ≤100 ≤100 ≤100 ≤100 Meaning ofabbreviations: SSt = standing sinter crucible; HST = hanging sintercrucible; HBt = Hanging metal sheet crucible; (W) = Crucible materialTungsten; TPM = Dew point measurement at gas outlet

TABLE 18 Example H5-1 H6-1 H7-1 H8-1 H8-2 H8-3 H8-4 H7-11 H7-12 H7-13H7-14 C content ppm <4 <4 <4 <4 <4 <4 <4  <4 <4 <4 <4 Cl content ppm100-200 100-200 100-200 100-200 100-200 100-200 100-200 <60 <60 300-400300-400 Al content ppb  20  20  20  20   20   20  20  20  20  20 20Total of the ppb <400 <400 <400 <400 <400 <400 <400  <900  <1200  <1200   <1200  concentrations of Ca, Co, Cr, Cu, Fe, Ge, Hf, K, Li, Mg,Mn, Mo, Na, Nb, Ni, Ti, V, W, Zn, Zr OH content ppm 400 400 400 250 400500 800 321 525 447 560 Alkaline earth ppb 115 115 115 115 115 115 115118 59 116 113 metal content ODC content 1/cm³ <4 * 10¹⁵ <4 * 10¹⁵ <4 *10¹⁵ <4 * 10¹⁵ <4 * 10¹⁵ <4 * 10¹⁵ <4 * 10¹⁵ 4 * 10¹⁵ 3 * 10¹⁵ 4 * 10¹⁵4 * 10¹⁵ Content of W, ppb <300 <300 <100 <50 <100 <5 100 347 1214 4691922 Mo, Re, Ir, Os ppb ppb ppb ppb ppb ppm ppm Outer diameter cm  26.0 19.7 19.7 19.7   19.7   19.7   19.7   19.7   19.7   19.7   19.7 oftubular thread/quartz glass body Viscosity lg(η/ @1250° C. dPas) 11.69 ±11.69 ± 11.69 ± 12.06 ± 11.69 ± 11.69 ± 11.63 ± 11.69 ± 11.69 ± 11.69 ±11.69 ± @1300° C. 0.13 0.13 0.13 0.15 0.13 0.13 0.13 0.13 0.14 0.16 0.16@1350° C. 11.26 ± 11.26 ± 11.26 ± 11.38 ± 11.26 ± 11.26 ± 11.22 ± 11.26± 11.26 ± 11.26 ± 11.26 ± 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.2 0.4 0.410.69 ± 10.69 ± 10.69 ± 10.75 ± 10.69 ± 10.69 ± 10.65 ± 10.69 ± 10.69 ±10.69 ± 10.69 ± 0.07 0.07 0.07 0.08 0.07 0.07 0.07 0.07 0.08 0.1 0.1

TABLE 19 Example H-7-1 H8-1 H8-2 H8-3 H8-4 Distributor cm    2 — — — —ring (Gas inlet in the melting crucible), Height above the glass meltLocation of In the lid In the lid In the lid In the In the gas outlet ofthe of the of the lid of lid of melting melting melting the the cruciblecrucible crucible melting melt- cruci- ing ble cruci- ble Dew point of °C. −90 −90 −90 −90 −90 the gas flow Before intro- duction into meltingcrucible After removal ° C. −10 −30 −10    0 +10 from melting crucible

I. Post Processing of a Quartz Glass Body

A quartz glass body obtained in example H1-1 and which has already beendrawn (1000 kg, Surface area=110 m²; Diameter=1.65 cm, Total length 2120m) is cut into pieces with a length of 200 cm by scoring and striking.The end surfaces were post worked by sawing to obtain a flat endsurface. The obtained batch of quartz glass bodies (I-1) was cleaned bydipping in an HF bath (V=2 m³) for 30 minutes and then rinsed with fullydesalinated water (to obtain quartz glass body (I-1′)).

J. “Used Acid” (HF Bath after Use)

The liquid in the dipping bath in example I (V=2 m³) is tested directlyafter the treatment of the quartz glass body (I-1′) and without furthertreatment. The liquid employed for the above described treatment ischaracterised before and after the treatment by the properties given inTable 20.

TABLE 20 Before After treatment of a treatment of quartz glass body of aquartz glass mass m = 1000 kg and Element Unit body surface area of 110m² Al ppm 0.04 0.8 Refractory metal (W, ppm 0 0.15 Mo, . . .) Furthermetals accord- ppm 0.15 1 ing to entire list * in total, of which Ca ppm0.01 0.3 Mg ppm 0.04 0.09 Na ppm 0.04 0.1 Cr ppm 0.01 0.01 Ni ppm 0.0010.01 Fe ppm 0.01 0.05 Zr ppm 0.01 0.05 Ti ppm 0.01 0.05 HF wt.-% 40 35Content of Si-F com- wt.-% 4 6 pounds Density g/cm³ 1.14 1.123

K. Making Quartz Glass Grain

Quartz glass bodies with the features as stated in Table 21 are reducedin size to give quartz glass grain, whereby 100 kg of the quartz glassbody is subjected to so-called electrodynamic size reduction, whereinthe original glass is reduced in size to the particle size desired byusing electrical pulses in a basin of water. If necessary, the materialis filtered using a vibrating filter to remove unwanted fine and coarsecomponents. The quartz glass grain is rinsed, acidized with HF, rinsedwith water again and dried. The cleaned quartz glass grain has thecharacteristics as stated in Table 22.

TABLE 21 Example H1-1 H4-1 C content Ppm <4 <4 Cl content Ppm <50 <50 Alcontent Ppb <40 <40 Total metal content except Al Ppb <1000 <1000 OHcontent Ppm 400 80 Viscosity Lg(η/dPas) @ 1250° C. 11.69 ± 0.13 12.16 ±0.2 @ 1300° C. 11.26 ± 0.1   11.49 ± 0.15 @ 1350° C. 10.69 ± 0.07 10.88± 0.1

TABLE 22 Example I1-1 I4-1 Educt = product from H1-1 H4-1 C content ppm<4 <4 Cl content ppm <50 <50 Al content ppb <40 <40 Total metal contentexcept Al ppb <1000 <1000 OH content Ppb 400 80 BET cm²/g <1 <1 Bulkdensity g/cm³ 1.25 1.35 Particle size D10 mm 0.85 0.09 D50 mm 2.21 0.18D90 mm 3.20 0.27

1. A process for the preparation of a quartz glass body comprising:providing a silicon dioxide granulate, wherein the silicon dioxidegranulate was made from pyrogenic silicon dioxide powder and the silicondioxide granulate comprises a BET surface area in a range from 20 to 40m₂/g; making a glass melt out of the silicon dioxide granulate in anoven; and making a quartz glass body out of at least part of the glassmelt; wherein the oven has at least a first and a further chamberconnected to one another by a passage; wherein the first and furtherchambers are at different temperatures; and wherein the temperature inthe first chamber is in a range of 1200 to 1800° C. lower than thetemperature in the further chamber.
 2. The process according to claim 1,wherein there is an additive in the first chamber selected from thegroup consisting of halogens, inert gas, base, oxygen or a combinationof two or more of them.
 3. The process according to claim 2, wherein thehalogen is selected from the group consisting of chlorine, fluorine,compounds containing chlorine, compounds containing fluorine and acombination of two or more thereof, and wherein the inert gas isselected from the group consisting of nitrogen, helium and a combinationof the two.
 4. The process according to claim 1, wherein in the firstchamber there is a pressure of less than 500 mbar.
 5. The processaccording to claim 1, wherein the silicon dioxide granulate comprises atleast one of: a mean particle size in a range from 50 to 500 μm a bulkdensity in a range from 0.5 to 1.2 g/cm3; a carbon content of less than10 ppm; an aluminium content of less than 200 ppb; a tamped density in arange from 0.7 to 1.2 g/cm3; a pore volume in a range from 0.1 to 2.5mL/g; an angle of repose in a range from 23 to 26° a particle sizedistribution D10 in a range from 50 to 150 μm; a particle sizedistribution D50 in a range from 150 to 300 μm; and a particle sizedistribution D90 in a range from 250 to 620 μm; wherein the ppm and ppbare each based on the total weight of the silicon dioxide powder.
 6. Theprocess according to claim 1, wherein the silicon dioxide is transportedfrom the first to the further chamber as granulate.
 7. The processaccording to claim 1, wherein the first chamber comprises at least oneelement selected from the group consisting of quartz glass, a refractorymetal, aluminium and a combination of two or more of them.
 8. Theprocess according to claim 1, wherein the further chamber is a crucibleof a metal sheet or a sinter material containing a sinter metal, whereinthe metal sheet or the sinter metal is selected from the groupconsisting of molybdenum, tungsten and a combination of them.
 9. Theprocess according to claim 1, wherein the BET surface area before makinga glass melt out of the silicon dioxide granulate in an oven is notreduced to less than 5 m2/g.
 10. The process according to claim 1,wherein melt energy is transmitted to the silicon dioxide granulate viaa solid surface.
 11. The process according to claim 1, wherein hydrogen,helium, nitrogen or a combination of two or more of them is present inthe gas space of the oven.
 12. The process according to claim 1, whereinproviding the silicon dioxide granulate comprises: providing silicondioxide powder comprising: a BET surface area in a range from 20 to 60m2/g; and a bulk density in a range from 0.01 to 0.3 g/cm3; processingthe silicon dioxide powder to obtain a silicon dioxide granulate;wherein the silicon dioxide granulate has a larger particle size thanthe silicon dioxide powder.
 13. The process according to claim 12,wherein the provided silicon dioxide powder comprises at least one of: acarbon content of less than 50 ppm a chlorine content of less than 200ppm; an aluminium content of less than 200 ppb; a total content ofmetals which are different from aluminium of less than 5 ppm; at least70 wt.-% of the powder particles have a primary particle size in a rangefrom 10 to 100 nm; a tamped density in a range from 0.001 to 1.3 g/cm3;a residual moisture content of less than 5 wt.-%; a particle sizedistribution D10 in the range from 1 to 7 μm; a particle sizedistribution D50 in the range from 6 to 15 μm; and a particle sizedistribution D90 in the range from 10 to 40 μm; wherein the wt.-%, theppm and the ppb are each based on the total weight of the sili-condioxide powder.
 14. The process according to claim 11, wherein thesilicon dioxide powder is made from an element selected from the groupconsisting of siloxanes, silicon alkoxides and silicon halides.
 15. Theprocess according to claim 11, further comprising forming a hollow bodywith at least one opening from the quartz glass body.
 16. A quartz glassbody obtained by a process according to claim
 11. 17. The quartz glassbody according to claim 16, comprising at least one of: an OH content ofless than 500 ppm; a chlorine content of less than 60 ppm; an aluminiumcontent of less than 200 ppb; an ODC content of less than 5*1015/cm3; ametal content of metals different from aluminium of less than 1 ppm; aviscosity (p=1013 hPa) in a range from log 10 (η(1250° C.)/dPas)=11.4 tolog 10 (η(1250° C.)/dPas)=12.9, or log 10 (η(1300° C.)/dPas)=11.1 to log10 (η(1300° C.)/dPas)=12.2, or log 10 (η(1350° C.)/dPas)=10.5 to log 10(η(1350° C.)/dPas)=11.5; a standard deviation of the OH content of notmore than 10%, based on the OH-content of the quartz glass body; astandard deviation of the Cl content of not more than 10%, based on theCl content of the quartz glass body; a standard deviation of the Alcontent of not more than 10%, based on the Al content of the quartzglass body; a refractive index homogeneity of less than 10-4; acylindrical form; a tungsten content of less than 1000 ppb; and amolybdenum content of less than 1000 ppb, wherein the ppb and ppm areeach based on the total mass of the quartz glass body.
 18. A process forthe preparation of a light guide comprising: providing a quartz glassbody according to the process of claim 1; process the quartz glass bodyto obtain a hollow body with at least two openings; introduce one ormultiple core rods into the quartz glass body through one of the atleast two openings to obtain a precursor; and drawing the precursor inthe warm to obtain the light guide with one or multiple cores and ajacket.
 19. A process for the preparation of an illuminant comprising:providing a quartz glass body according to the process of claim 1;processing the quartz glass body to obtain a hollow body; fitting thehollow body with electrodes; and filling the hollow body with a gas. 20.A process for the preparation of a formed body comprising: providing aquartz glass body according to claim 16; and forming the formed body outof the quartz glass body.